WO2022166314A1 - 改性珠光粉体及其制备方法、化妆品 - Google Patents
改性珠光粉体及其制备方法、化妆品 Download PDFInfo
- Publication number
- WO2022166314A1 WO2022166314A1 PCT/CN2021/132080 CN2021132080W WO2022166314A1 WO 2022166314 A1 WO2022166314 A1 WO 2022166314A1 CN 2021132080 W CN2021132080 W CN 2021132080W WO 2022166314 A1 WO2022166314 A1 WO 2022166314A1
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- Prior art keywords
- powder
- pearlescent powder
- modified
- pearlescent
- fluorine
- Prior art date
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Definitions
- the present application relates to the technical field of cosmetics, in particular to modified pearlescent powder, a preparation method thereof, and cosmetics.
- Pearlescent powder is widely used in the cosmetic industry because of its unique luster, and it is the most important colorant in cosmetic cosmetics for face, lips, eyes and nails.
- traditional pearlescent powders also have some problems, such as: pearlescent powders with a particle size less than or equal to 60 microns are not shiny enough, while pearlescent powders with a particle size larger than 60 microns are not skin-friendly and soft enough.
- all pearlescent powders are hydrophilic and lipophilic, which makes it difficult for traditional cosmetics to spread evenly on the skin and has poor makeup retention.
- a modified pearlescent powder the modified pearlescent powder comprises a pearlescent powder, a lauroyl lysine powder covered on the surface of the pearlescent powder, and a containing compound connected to the pearlescent powder through a covalent bond. Fluorosilane coupling agent.
- the lauroyl lysine powder has a sheet-like structure.
- some of the fluorine-containing silane coupling agents associate with each other and form a network structure.
- the mass of the fluorine-containing silane coupling agent is 0.1%-10.0% of the mass of the pearlescent powder
- the mass of the lauroyl lysine powder is the mass of the pearlescent powder 0.1%-10.0% of mass.
- the general formula of the fluorine-containing silane coupling agent is R-Si-(OC m H 2m+1 ) 3 , where R is C n F 2n+1 -(CH 2 ) 2 -, 1 ⁇ n ⁇ 6, n is an integer, m is 1 or 2.
- the fluorine-containing silane coupling agent includes at least one of perfluorooctyltriethoxysilane, tridecafluorooctyltrimethoxysilane, and heptadecafluorodecyltrimethoxysilane .
- a method for preparing the modified pearlescent powder as described above comprises: mixing the pearlescent powder, the fluorine-containing silane coupling agent and the lauroyl lysine powder, and heating to obtain the modified pearlescent powder.
- the heating temperature is 100°C-120°C, and the heating time is 1 hour-3 hours.
- a cosmetic comprising the modified pearlescent powder as described above.
- the modified pearlescent powder is directionally distributed in the cosmetic.
- the pearlescent powder is chemically and physically modified by using fluorine-containing silane coupling agent and lauroyl lysine powder, so that the obtained modified pearlescent powder is more soft and skin-friendly, and at the same time,
- the surface tension of the modified pearlescent powder is extremely low, and it has the effect of hydrophobic and oleophobic. It can not only make the modified pearlescent powder form a mirror effect in cosmetics and show higher gloss, but also can effectively improve the use of the modified pearlescent powder.
- the spreadability of powdered cosmetics enables the cosmetics to be applied evenly on the skin and has better longevity.
- Example 1 is a SEM image of the surface of the pearlescent powder covered by the lauroyl lysine powder in the modified pearlescent powder obtained in Example 1.
- Figure 2 is a diagram showing the effect of dispersing the pearlescent powder of Example 1 and the obtained modified pearlescent powder in glycerol.
- FIG. 3 is an effect diagram of applying the modified pearlescent powder dispersed in glycerin and the pearlescent powder dispersed in glycerin on the skin.
- FIG. 4 is an effect diagram of the modified pearlescent powder obtained in Example 1 dispersed in water.
- FIG. 5 is an effect diagram of applying the eye shadows obtained by applying Example 1-1 and applying Comparative Example 1-1 to the skin.
- the modified pearlescent powder provided by the present application, the preparation method thereof, and the cosmetic will be further described below.
- the modified pearlescent powder provided in this application is mainly used in cosmetics to improve the gloss, skin-friendly and long-lasting properties of cosmetics.
- the modified pearlescent powder includes a pearlescent powder, a lauroyl lysine powder covering the surface of the pearlescent powder, and a fluorine-containing silane coupling agent connected to the pearlescent powder through a covalent bond .
- the pearlescent powder has a layered structure, including a substrate and a cover layer
- the substrate includes a mica substrate, a silica substrate, an aluminum substrate, a glass substrate, an oxide substrate, a kaolin substrate, and a ceramic substrate.
- At least one of a substrate and a graphite substrate, and the cover layer includes at least one of a titanium dioxide cover layer, an iron oxide cover layer, a CI 77510 (pigment blue 27, ferric ferrocyanide) cover layer, and a carmine red cover layer. kind.
- the pearlescent powder can be selected from mica titanium pearlescent Powder, the substrate is a mica substrate, and the covering layer is a titanium dioxide covering layer.
- the general formula of the fluorine-containing silane coupling agent is R-Si-(OC m H 2m+1 ) 3 , where R is C n F 2n+1 -(CH 2 ) 2- , 1 ⁇ n ⁇ 6, n is an integer, m is 1 or 2.
- the fluorine-containing silane coupling agent connected to the pearlescent powder by covalent bond is hydrolyzed by the alkoxy group of the fluorine-containing silane coupling agent to form silanol, and the silanol reacts with the hydroxyl group on the surface of the pearlescent powder to form a hydrogen bond and dehydrate obtained by condensation.
- the fluorine-containing silane coupling agent connected to the pearlescent powder through a covalent bond is a fluorine-containing segment, and the fluorine-containing segment at least includes a segment whose structural formula is shown in formula (1):
- the surface tension of the modified pearlescent powder is extremely low after the surface of the pearlescent powder is connected with a fluorine-containing silane coupling agent through covalent bonds, which in turn makes the modified pearlescent powder have a hydrophobic and hydrophobic property. oil effect.
- some of the fluorine-containing silane coupling agents associate with each other and form a network structure, and the network structure covers the surface of the pearlescent powder to form a film layer.
- the mass of the fluorine-containing silane coupling agent is 0.1%-10.0% of the mass of the pearlescent powder, optionally 1.5% -3%.
- the fluorine-containing silane coupling agent comprises at least one of perfluorooctyltriethoxysilane, tridecafluorooctyltrimethoxysilane, and heptadecafluorodecyltrimethoxysilane, Optionally, perfluorooctyltriethoxysilane.
- Lauroyl lysine powder is an amino acid derivative, which has the effect of being soft and sticking to the skin. Therefore, after covering the lauroyl lysine powder on the pearlescent powder, it can give the modified pearlescent powder more softness and softness. Skin-friendly effect.
- the mass of the lauroyl lysine powder is 0.1%-10.0% of the mass of the pearlescent powder, Optional 3%-7%.
- the lauroyl lysine powder is mainly coated on the surface of the pearlescent powder by the physical action of van der Waals force.
- the network structure can also play the role of The function of fixing lauroyl lysine powder makes the combination of lauroyl lysine powder and pearl powder more reliable.
- the lauroyl lysine powder can be optionally in a sheet-like structure.
- the lamellar structure of laurel The size of the acyl-lysine powder is smaller than that of the pearlescent powder.
- the lauroyl lysine powder with an optional sheet-like structure and the segments of the fluorine-containing silane coupling agent are distributed in a staggered manner.
- the pearlescent powder is chemically and physically modified by using a fluorine-containing silane coupling agent and lauroyl lysine powder to make the modified pearlescent powder softer and more skin-friendly.
- the modified pearlescent powder is The surface tension of the powder is extremely low, and it has the effect of hydrophobic and oleophobic.
- the present application also provides a method for preparing the modified pearlescent powder, including: mixing the pearlescent powder, the fluorine-containing silane coupling agent and the lauroyl lysine powder, and heating to obtain the modified pearlescent powder.
- the pearlescent powder and the lauroyl lysine powder are mixed first, and then the fluorine-containing silane is added for coupling In order to avoid premature hydrolysis of the fluorine-containing silane coupling agent and connect it to the surface of the pearlescent powder, it will affect the coating effect of the lauroyl lysine powder on the surface of the pearlescent powder.
- the lauroyl lysine powder is randomly coated on the surface of the pearlescent powder, and then the fluorine-containing silane coupling agent reacts with the uncoated surface, and the fluorine-containing segment is modified on the pearlescent powder by covalent bonds.
- the surface of lauroyl lysine powder and the segments of the fluorine-containing silane coupling agent are interdigitated with each other.
- the heating temperature is 100°C-120°C, and the time is 1 hour-3 hours.
- the alkoxy group of the fluorine-containing silane coupling agent is hydrolyzed to form silanol, and the silanol reacts with the hydroxyl group on the surface of the pearlescent powder to form hydrogen bonds and dehydrate and condense to obtain the fluorine-containing silane coupling agent.
- the acyl-lysine powder is coated on the surface of the pearlescent powder by the physical action of van der Waals force.
- the present application can obtain the modified pearlescent powder which is more soft and skin-friendly, and has the effect of hydrophobic and oleophobic at the same time through the dry process.
- the method is simple and more suitable for industrial production.
- the layered pearlescent powder will inevitably be broken into smaller particle size pearlescent powder. It can be understood that it will reduce the pearlescent effect, color effect and goniochromatic effect.
- the pearlescent effect and color effect of the modified pearlescent powder obtained by modifying the fluorine-containing silane coupling agent and lauroyl lysine powder And the goniochromatic effect is still improved compared with the unmixed pearl powder.
- the present application also provides a cosmetic comprising the modified pearlescent powder as described above.
- the spreadability of the cosmetic using the modified pearlescent powder can be effectively improved, so that the cosmetic can be better spread evenly on the skin , and the makeup lasts better.
- the modified pearlescent powder can be directionally distributed in the cosmetic to form a mirror effect, so that the cosmetic exhibits higher gloss.
- modified pearlescent powder when the modified pearlescent powder is directionally distributed in cosmetics, it does not mean that the arrangement angles of the modified pearlescent powder are completely consistent, but tend to be consistent.
- the cosmetics include pressed powder products, all-water products, all-oil products, emulsified products, and the like.
- the liquid eye shadow includes the modified pearlescent powder as described above, and the mass percentage of the modified pearlescent powder in the liquid eye shadow is 1%-40%, optionally 10%- 20%.
- the liquid eye shadow also includes 35%-90% by mass of water, less than or equal to 20% by mass of polyol, less than or equal to 2% by mass of thickener, and less than or equal to 2% by mass % of emulsifier, 0.5%-1% of preservative by mass, and less than or equal to 2% of film-forming agent by mass.
- the polyol includes at least one of glycerol, propylene glycol, and butanediol
- the thickener includes at least one of xanthan gum, carbopol, hectorite, magnesium aluminum silicate, and cellulose
- the emulsifier includes at least one of polysorbate-80, polysorbate-60, PEG-80 sorbitan laurate, and PEG-7 glycerol cocoate
- the preservative includes benzene At least one of a mixture of oxyethanol and ethylhexylglycerol, a mixture of caprylyl glycol and ethylhexylglycerol, and ethylhexylglycerol
- the film-forming agent includes at least one of polyurethanes and polyacrylate copolymers kind.
- the surface tension of the modified pearlescent powder is extremely low and has the effect of hydrophobic and oleophobic, the overall surface energy of the liquid eye shadow is reduced, so that the liquid eye shadow has better spreadability and film-forming properties during application, and The liquid eyeshadows have better makeup hold.
- the modified pearlescent powder can be directionally distributed in the liquid eye shadow to form a mirror effect, so the liquid eye shadow can exhibit higher gloss.
- modified pearlescent powder its preparation method and cosmetics will be further described by the following specific examples.
- the lauroyl lysine powder with a sheet-like structure covers the surface of the pearlescent powder.
- the fluorine-containing silane coupling agent is connected to the pearlescent powder through covalent bonds, and part of the fluorine-containing silane coupling agent associates with each other to form a film with a network structure. Acyl-lysine powder and fluorine-containing silane coupling agent are distributed alternately.
- the pearlescent powder of this embodiment and the obtained modified pearlescent powder are dispersed in glycerol, as shown in Figure 2, the left side is the dispersion effect diagram of the modified pearlescent powder, and the right side is the dispersion effect diagram of the pearlescent powder , it can be seen from Figure 2 that since the modified pearlescent powder can be directionally distributed in glycerol to form a mirror effect, the modified pearlescent powder dispersed in glycerol on the left can show higher gloss.
- the left side is the smear effect of the modified pearlescent powder
- the right side is the pearlescent powder
- the surface tension of the modified pearlescent powder is extremely low, it has a hydrophobic and oleophobic effect, and the pearlescent powder is hydrophilic and lipophilic, so the modified pearlescent powder dispersed in glycerol Powders show better spreadability when applied, while pearlescent powders dispersed in glycerin shrink when applied.
- the modified pearlescent powder obtained in this example is dispersed in water, as shown in Figure 4, the surface energy of the modified pearlescent powder is low, and tends to be aligned on the surface of the polar system, forming a mirror effect, which can be compared Bright metallic luster.
- Example 2 The only difference between Example 2 and Example 1 is that the particle size of the pearlescent powder in Example 2 is 30 ⁇ m-150 ⁇ m.
- Example 3 The only difference between Example 3 and Example 2 is that the substrate of the pearlescent powder in Example 3 is a glass substrate.
- Example 4 The only difference between Example 4 and Example 1 is that the coating layers of the pearlescent powder in Example 4 are iron oxide and titanium dioxide, and the color of the pearlescent powder is gold.
- Example 5 The only difference between Example 5 and Example 1 is that the coating layer of the pearlescent powder in Example 5 is iron oxide, and the color of the pearlescent powder is reddish-brown.
- Example 6 The only difference between Example 6 and Example 1 is that the covering layer of the pearlescent powder in Example 6 is an organic lake and titanium dioxide, and the color of the pearlescent powder is rose red.
- Example 7 The only difference between Example 7 and Example 1 is that the mass of the lauroyl lysine powder with a sheet-like structure in Example 7 is 1 g.
- Example 8 The only difference between Example 8 and Example 1 is that the mass of the lauroyl lysine powder with a sheet-like structure in Example 8 is 100 g.
- Example 9 The only difference between Example 9 and Example 1 is that the mass of perfluorooctyltriethoxysilane in Example 9 is 1 g.
- Example 10 The only difference between Example 10 and Example 1 is that the mass of perfluorooctyltriethoxysilane in Example 10 is 100 g.
- Comparative Example 1 The only difference between Comparative Example 1 and Example 1 is that no perfluorooctyltriethoxysilane was added during the mixing process of Comparative Example 1.
- Comparative Example 2 The only difference between Comparative Example 2 and Example 1 is that no lauroyl lysine powder was added during the mixing process of Comparative Example 2.
- the pearlescent powder of each example and the modified pearlescent powder obtained in each example and comparative example were dispersed in water and white oil to determine the dispersibility. The results are shown in Table 1.
- the eye shadow includes phase A, phase B and phase C, wherein phase A includes mica, talc, silica, methyl methacrylate cross-linked polymer, magnesium myristate, magnesium stearate, and phase B includes poly Dimethicone, caprylic/capric triglyceride, isononyl isononanoate, VP/hexadecene copolymer, and the C phase is the modified pearlescent powder of Example 1.
- the mass percentage of mica is 50%
- the mass percentage of talc is 20%
- the mass percentage of silica is 5%
- the mass percentage of methyl methacrylate cross-linked polymer is 3%
- nutmeg The mass percentage of magnesium acid is 1%
- the mass percentage of magnesium stearate is 1%
- the mass percentage of polydimethylsiloxane is 3%
- the mass percentage of caprylic/capric triglyceride is 2%
- isononyl The mass percentage of isononyl acid is 2%
- the mass percentage of VP/hexadecene copolymer is 1%
- the mass percentage of modified pearlescent powder is 12%.
- phase A When preparing, first add phase A into the mixing pot and stir evenly at high speed, then mix phase B and add it to phase A and continue to stir evenly at high speed, then add phase C into the well-mixed phases A and B, and mix at low speed evenly. Finally, the material is discharged, pressed and formed to obtain eye shadow.
- compositions and mass percentages of application examples 1-2 to 1-6 refer to application example 1-1, the difference is that the C phase uses the modified pearlescent powder of example 2-6 respectively.
- compositions and mass percentages of application comparative examples 1-1 to 1-6 refer to application example 1-1, the difference is that the pearlescent powder of example 1-6 is used for the C phase.
- compositions and mass percentages of Application Comparative Examples 1-7 to 1-8 refer to Application Example 1-1, the difference is that the C phase uses the modified pearlescent powder of Comparative Example 1-2 respectively.
- the eye shadows obtained by the application example 1-1 and the application example 1-1 were applied to the skin, and the results are shown in Figure 5.
- the right side is the application effect of the eye shadow of the application example 1-1
- the left side is the application
- the smearing effect of the eye shadow of the ratio 1-1 can be seen from FIG. 5 , the eye shadow using the modified pearlescent powder of the present application has better spreadability, better adhesion to the skin, and better makeup retention.
- the liquid eye shadow includes deionized water, glycerin, xanthan gum, O/W emulsifier, polyurethane, and the modified pearlescent powder of Example 1. Based on the total mass of 100%, the mass percentage of deionized water is 67.5%, the mass percentage of glycerol is 10%, the mass percentage of xanthan gum is 0.5%, and the mass percentage of O/W emulsifier is 1.5%, Example 1 The mass percentage of modified pearlescent powder is 20%, and the mass percentage of polyurethane is 0.5%.
- compositions and mass percentages of application examples 2-2 to 2-6 refer to application example 2-1, the difference is that the modified pearlescent powder of example 2-6 is used respectively.
- compositions and mass percentages of application examples 2-1 to 2-6 refer to application example 2-1, the difference is that the pearlescent powders of examples 1-6 are respectively used.
- compositions and mass percentages of Application Comparative Examples 2-7 to 2-8 refer to Application Example 2-1, the difference is that the modified pearlescent powder of Comparative Example 1-2 is used respectively.
- Phase A includes polydimethylsiloxane, isododecane, cyclopentasiloxane, distearyldimethicone Ammonium Hectorite, Phenyl Trimethicone, PEG-10 Dimethicone, Caprylic/Capric Triglyceride, Trimethylsiloxysilicate, Polymethylsiloxane Hemioxane, phase B includes water and alcohol, and phase C is the modified pearlescent powder of Example 1.
- the mass percentage of polydimethylsiloxane is 9%, the mass percentage of isododecane is 14.3%, the mass percentage of cyclopentasiloxane is 20%, the dihard The mass percentage of tallow dimethylammonium hectorite is 0.7%, the mass percentage of phenyl trimethicone is 6%, the mass percentage of PEG-10 polydimethylsiloxane is 3%, and the caprylic acid/ The mass percentage of capric triglyceride is 5%, the mass percentage of trimethylsiloxysilicate is 2%, the mass percentage of polymethylsilsesquioxane is 5%, and the mass percentage of water is 5% , the mass percentage of alcohol is 12%, and the mass percentage of modified pearlescent powder is 18%.
- phase A When preparing, first add phase A into the beaker, stir evenly at medium speed, then mix phase B and then add it to phase A and homogenize for 10 minutes, then add phase C into the well-mixed phase A and phase B, and mix at low speed to obtain A highlighter.
- compositions and mass percentages of application examples 3-2 to 3-6 refer to application example 3-1, the difference is that the C phase uses the modified pearlescent powder of example 2-6 respectively.
- compositions and mass percentages of application examples 3-1 to 3-6 refer to application example 3-1, the difference is that the pearlescent powders of examples 1-6 are respectively used for the C phase.
- compositions and mass percentages of Application Comparative Examples 3-7 to 3-8 refer to Application Example 3-1, the difference is that the C phase uses the modified pearlescent powder of Comparative Example 1-2 respectively.
- High-light brightening liquid (W/O type): This emulsified product includes A phase, B phase, C phase and D phase, wherein, A phase includes PEG-10 polydimethylsiloxane, lauryl PEG-9 poly Dimethicone Dimethicone, Phenyl Trimethicone, Caprylic/Capric Triglyceride, Octyldodecanol, Butylene Glycol Dicaprylic/Dicaprate, Trimethylsiloxysilicate and/or Dimethicone, C9-12 Alkane, Phase B including Cyclopentasiloxane, Distearyl Dimethylammonium Hectorite, C The phase includes water, glycerin, magnesium sulfate, propylene glycol, phenoxyethanol/ethylhexylglycerol, and phase D is the modified pearlescent powder of Example 1.
- a phase includes PEG-10 polydimethylsiloxane, lauryl PEG-9 poly Dimethi
- the mass percentage of PEG-10 polydimethylsiloxane is 2%, and the mass percentage of lauryl PEG-9 polydimethylsiloxyethyl polydimethylsiloxane is 1% , the mass percentage of phenyl trimethicone is 7%, the mass percentage of caprylic/capric triglyceride is 4%, the mass percentage of octyldodecanol is 5%, butanediol dicaprylic acid/di
- the mass percentage of caprate is 5%, the mass percentage of trimethylsiloxysilicate is 2%, the mass percentage of C9-12 alkane is 6%, and the mass percentage of cyclopentasiloxane is 15%, the mass percentage of distearyl dimethylammonium hectorite is 1%, the mass percentage of water is 30.55%, the mass percentage of glycerol is 5%, the mass percentage of magnesium sulfate is 0.7%, and the
- phase A When preparing, first add phase A into the beaker, stir and disperse evenly at 60°C, then mix phase B and add it to phase A and homogenize for 5 minutes, then add phase C while homogenizing, and then homogenize for 5 minutes after adding phase C. , and then add phase D into the well-mixed phase A, phase B and phase C, and mix uniformly at low speed to obtain a high-gloss brightening liquid (W/O type).
- W/O type high-gloss brightening liquid
- compositions and mass percentages of application examples 4-2 to 4-6 refer to application example 4-1, the difference is that the modified pearlescent powder of example 2-6 is used for the D phase.
- compositions and mass percentages of application examples 4-1 to 4-6 refer to application example 4-1, the difference is that the pearlescent powders of examples 1-6 are respectively used in the D phase.
- compositions and mass percentages of Application Comparative Examples 4-7 to 4-8 refer to Application Example 3-1, the difference is that the C phase uses the modified pearlescent powder of Comparative Example 1-2 respectively.
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Abstract
一种改性珠光粉体及其制备方法，所述改性珠光粉体包括珠光粉体、覆盖于所述珠光粉体表面的月桂酰赖氨酸粉体以及通过共价键连接于所述珠光粉体的含氟硅烷偶联剂。还涉及一种化妆品，所述化妆品包括所述的改性珠光粉体。
Description
相关申请
本申请要求2021年2月5日申请的，申请号为202110162074.5，发明名称为“改性珠光粉体及其制备方法、化妆品”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
本申请涉及化妆品技术领域，特别是涉及改性珠光粉体及其制备方法、化妆品。
珠光粉体因为其独特的光泽而被广泛应用于化妆品行业，是面部、唇、眼和指甲用美容化妆品中最重要的着色剂。但是，传统的珠光粉体也存在一些问题，如：粒径小于或等于60微米的珠光粉体不够闪亮，而粒径大于60微米的珠光粉体不够贴肤和柔软。另外，所有的珠光粉体均是亲水亲油的，导致传统的化妆品在肌肤上不易涂抹均匀，且持妆性欠佳。
发明内容
基于此，有必要针对上述问题，提供一种更加柔软和贴肤，同时具有疏水疏油的效果的改性珠光粉体及其制备方法，以及应用所述改性珠光粉体的化妆品。
一种改性珠光粉体，所述改性珠光粉体包括珠光粉体、覆盖于所述珠光粉体表面的月桂酰赖氨酸粉体以及通过共价键连接于所述珠光粉体的含氟硅烷偶联剂。
在其中一个实施例中，所述月桂酰赖氨酸粉体为片状结构。
在其中一个实施例中，部分所述含氟硅烷偶联剂相互缔和形成网状结构。
在其中一个实施例中，所述含氟硅烷偶联剂的质量为所述珠光粉体的质量的0.1％-10.0％，所述月桂酰赖氨酸粉体的质量为所述珠光粉体的质量的0.1％-10.0％。
在其中一个实施例中，所述含氟硅烷偶联剂的通式为R-Si-(OC
mH
2m+1)
3，式中，R为C
nF
2n+1-(CH
2)
2-，1≤n≤6，n为整数，m为1或2。
在其中一个实施例中，所述含氟硅烷偶联剂包括全氟辛基三乙氧基硅烷、十三氟辛基三甲氧基硅烷、十七氟癸基三甲氧基硅烷中的至少一种。
一种如上所述改性珠光粉体的制备方法，包括：将珠光粉体、含氟的硅烷偶联剂以及月桂酰赖氨酸粉体混合，加热，得到改性珠光粉体。
在其中一个实施例中，所述加热的温度为100℃-120℃，时间为1小时-3小时。
一种化妆品，所述化妆品包括如上所述的改性珠光粉体。
在其中一个实施例中，所述改性珠光粉体于所述化妆品中定向分布。
本申请中，通过使用含氟的硅烷偶联剂以及月桂酰赖氨酸粉体对珠光粉体进行化学和物理的改性处理，使获得的改性珠光粉体更加柔软和贴肤，同时，改性珠光粉体的表面张力极低，具有疏水疏油的效果，既可以使改性珠光粉体在化妆品中形成镜面效应，表现出更高的光泽度，又能够有效改善使用该改性珠光粉体的化妆品的铺展性，使得化妆品在肌肤上能够更好的涂抹均匀，且持妆性更好。
图1为实施例1获得的改性珠光粉体中月桂酰赖氨酸粉体覆盖于珠光粉体的表面的SEM图。
图2为实施例1的珠光粉体以及获得的改性珠光粉体分散于甘油中的效 果图。
图3为将分散于甘油中的改性珠光粉体以及分散于甘油中的珠光粉体涂抹于皮肤上的效果图。
图4为实施例1获得的改性珠光粉体分散于水中的效果图。
图5为应用实施例1-1和应用对比例1-1获得的眼影刷于皮肤上的效果图。
以下将对本申请提供的改性珠光粉体及其制备方法、化妆品作进一步说明。
本申请提供的改性珠光粉体主要应用于化妆品中，用以改善化妆品的光泽度、亲肤性以及持妆性。
具体地，所述改性珠光粉体包括珠光粉体、覆盖于所述珠光粉体表面的月桂酰赖氨酸粉体以及通过共价键连接于所述珠光粉体的含氟硅烷偶联剂。
其中，所述珠光粉体为层状结构，包括衬底和覆盖层，所述衬底包括云母衬底、硅石衬底、铝衬底、玻璃衬底、氧化物衬底、高岭土衬底、陶瓷衬底、石墨衬底中的至少一种，所述覆盖层包括二氧化钛覆盖层、氧化铁覆盖层、CI 77510(颜料蓝27，亚铁氰化铁)覆盖层、胭脂红覆盖层中的至少一种。
由于二氧化钛和云母的折射率不同，通过光线的多重反射与干涉作用能够产生较好的珠光效应、色彩效应和视角闪色效应，在一实施方式中，所述珠光粉体可选为云母钛珠光粉体，其衬底为云母衬底，覆盖层为二氧化钛覆盖层。
本申请的改性珠光粉体中，所述含氟硅烷偶联剂的通式为 R-Si-(OC
mH
2m+1)
3，式中，R为C
nF
2n+1-(CH
2)
2-，1≤n≤6，n为整数，m为1或2。通过共价键连接于所述珠光粉体的含氟硅烷偶联剂为由含氟硅烷偶联剂的烷氧基水解形成硅醇，硅醇与珠光粉体表面的羟基反应形成氢键并脱水缩合得到。更具体的讲，通过共价键连接于所述珠光粉体的含氟硅烷偶联剂为含氟链段，所述含氟链段至少包括结构式如式(1)所示的链段：
由于氟的表面能低，所以，珠光粉体的表面通过共价键连接有含氟硅烷偶联剂后，使得改性珠光粉体的表面张力极低，进而使得改性珠光粉体具有疏水疏油的效果。
在一实施方式中，部分所述含氟硅烷偶联剂相互缔和形成网状结构，该网状结构覆盖于珠光粉体的表面，形成膜层。
为了使改性珠光粉体具有疏水疏油的效果，在一实施方式中，所述含氟硅烷偶联剂的质量为所述珠光粉体的质量的0.1％-10.0％，可选为1.5％-3％。
在一实施方式中，所述含氟硅烷偶联剂包括全氟辛基三乙氧基硅烷、十三氟辛基三甲氧基硅烷、十七氟癸基三甲氧基硅烷中的至少一种，可选为全氟辛基三乙氧基硅烷。
月桂酰赖氨酸粉体是一种氨基酸衍生物，具有柔性贴肤的效果，因此，于珠光粉体上覆盖所述月桂酰赖氨酸粉体后，可以赋予改性珠光粉体更加柔软和贴肤的效果。
为了使改性珠光粉体具有较佳的柔软和贴肤的效果，在一实施方式中，所述月桂酰赖氨酸粉体的质量为所述珠光粉体的质量的0.1％-10.0％，可选为3％-7％。
月桂酰赖氨酸粉体主要通过范德华力的物理作用包覆于珠光粉体的表面，当部分所述含氟硅烷偶联剂相互缔和形成网状结构时，该网状结构也可以起到固定月桂酰赖氨酸粉体的作用，使月桂酰赖氨酸粉体与珠光粉体的结合更可靠。
为了使改性珠光粉体具有更加柔软和贴肤的效果，在一实施方式中，所述月桂酰赖氨酸粉体可选为片状结构。
进一步地，为了使改性珠光粉体具有更好的珠光效应、色彩效应和视角闪色效应，疏水疏油的效果以及柔软和贴肤的综合效果，在一实施方式中，片状结构的月桂酰赖氨酸粉体的尺寸小于珠光粉体的尺寸。同时，可选片状结构的月桂酰赖氨酸粉体与含氟硅烷偶联剂的链段相互交错分布。
因此，本申请通过使用含氟硅烷偶联剂以及月桂酰赖氨酸粉体对珠光粉体进行化学和物理的改性处理，使改性珠光粉体更加柔软和贴肤，同时，改性珠光粉体的表面张力极低，具有疏水疏油的效果。
本申请还提供一种如上所述改性珠光粉体的制备方法，包括：将珠光粉体、含氟硅烷偶联剂以及月桂酰赖氨酸粉体混合，加热，得到改性珠光粉体。
由于含氟硅烷偶联剂在空气中烷氧基就会水解形成硅醇，所以，在一实施方式中，先将珠光粉体与月桂酰赖氨酸粉体混合，再加入含氟硅烷偶联剂，以避免含氟硅烷偶联剂过早水解而连接于珠光粉体的表面，影响月桂酰赖氨酸粉体在珠光粉体表面的包覆效果。
同时，月桂酰赖氨酸粉体先随机包覆于珠光粉体的表面，然后含氟硅烷偶联剂再与未包覆的表面进行反应，含氟链段通过共价键修饰于珠光粉体的表面，从而，使得月桂酰赖氨酸粉体与含氟硅烷偶联剂的链段相互交错分布。
在一实施方式中，所述加热的温度为100℃-120℃，时间为1小时-3小 时。在所述加热的过程中，含氟硅烷偶联剂的烷氧基水解形成硅醇，硅醇与珠光粉体表面的羟基反应形成氢键并脱水缩合得到含氟硅烷偶联剂，同时，月桂酰赖氨酸粉体通过范德华力的物理作用而包覆于珠光粉体的表面。
因此，本申请通过干法工艺即可制得更加柔软和贴肤，同时具有疏水疏油的效果的改性珠光粉体，方法简单，更适用于工业化生产。
在将珠光粉体、含氟硅烷偶联剂以及月桂酰赖氨酸粉体进行混合的过程中，层状结构的珠光粉体不可避免的会被打碎成更小粒径的珠光粉体，可以理解，其会降低珠光效应、色彩效应和视角闪色效应，但是，通过含氟硅烷偶联剂以及月桂酰赖氨酸粉体改性后获得的改性珠光粉体的珠光效应、色彩效应和视角闪色效应相较于未混合前的珠光粉体而言仍然有所提高。
本申请还提供一种化妆品，所述化妆品包括如上所述的改性珠光粉体。
由于改性珠光粉体的表面张力极低，具有疏水疏油的效果，所以，能够有效改善使用该改性珠光粉体的化妆品的铺展性，使得所述化妆品在肌肤上能够更好的涂抹均匀，且持妆性更好。
同时，所述改性珠光粉体能够于所述化妆品中定向分布，形成镜面效应，以使所述化妆品表现出更高的光泽度。
应予说明的是，改性珠光粉体在化妆品中定向分布时，并不是指改性珠光粉体的排列角度完全一致，而是趋于一致。
在一实施方式中，所述化妆品包括压粉类产品、全水型产品、全油型产品、乳化型产品等。
以液体眼影为例，所述液体眼影包括如上所述的改性珠光粉体，所述改性珠光粉体在所述液体眼影中的质量百分数为1％-40％，可选为10％-20％。
另外，所述液体眼影中还包括有质量百分数为35％-90％的水，质量百分 数小于或等于20％的多元醇，质量百分数小于或等于2％的增稠剂，质量百分数小于或等于2％的乳化剂，质量百分数为0.5％-1％的防腐剂，质量百分数小于或等于2％的成膜剂。
其中，所述多元醇包括甘油、丙二醇、丁二醇中的至少一种，所述增稠剂包括黄原胶、卡波、水辉石、硅酸铝镁、纤维素中的至少一种，所述乳化剂包括聚山梨醇酯-80、聚山梨醇酯-60、PEG-80失水山梨醇月桂酸酯、PEG-7甘油椰油酸酯中的至少一种，所述防腐剂包括苯氧乙醇与乙基己基甘油的混合物、辛甘醇与乙基己基甘油的混合物、乙基己基甘油中的至少一种，所述成膜剂包括聚氨酯类、聚丙烯酸酯共聚物类中的至少一种。
由于改性珠光粉体的表面张力极低，具有疏水疏油的效果，因此，降低了所述液体眼影整体的表面能，使得液体眼影在涂抹时铺展性和成膜性更好，以及，使得所述液体眼影具有更好的持妆性。
同时，所述改性珠光粉体能够于液体眼影中定向分布，形成镜面效应，因此，所述液体眼影能够表现出更高的光泽度。
以下，将通过以下具体实施例对所述改性珠光粉体及其制备方法、化妆品做进一步的说明。
实施例1
将30g片状结构的月桂酰赖氨酸粉体与1kg的珠光粉体(10μm-60μm，银白色，衬底为云母，覆盖层为二氧化钛)混合均匀，然后加入10g全氟辛基三乙氧基硅烷混合均匀，加热至110℃保温2小时，得到改性珠光粉体。
如图1所示，该实施例获得的改性珠光粉体中，片状结构的月桂酰赖氨酸粉体覆盖于珠光粉体的表面。另外，改性珠光粉体中，含氟硅烷偶联剂通过共价键连接于珠光粉体，且部分含氟硅烷偶联剂相互缔和形成网状结构的 膜，其中，片状结构的月桂酰赖氨酸粉体与含氟硅烷偶联剂相互交错分布。
将该实施例的珠光粉体以及获得的改性珠光粉体分散于甘油中，如图2所示，左侧为改性珠光粉体的分散效果图，右侧为珠光粉体的分散效果图，由图2可知，由于改性珠光粉体能够于甘油中定向分布，形成镜面效应，所以左侧分散于甘油中的改性珠光粉体能够表现出更高的光泽度。
将分散于甘油中的改性珠光粉体以及分散于甘油中的珠光粉体涂抹于皮肤上，如图3所示，左侧为改性珠光粉体的涂抹效果图，右侧为珠光粉体的涂抹效果图，由图3可知，由于改性珠光粉体的表面张力极低，具有疏水疏油的效果，而珠光粉体是亲水亲油的，所以，分散于甘油中的改性珠光粉体在涂抹时能够展现出更好的铺展性，而分散于甘油中的珠光粉体在涂抹时会收缩。
将该实施例获得的改性珠光粉体分散于水中，如图4所示，改性珠光粉体的表面能较低，在极性体系的表面倾向于定向排列，形成镜面效应，能够表现比较亮的金属光泽感。
实施例2
实施例2与实施例1的区别仅在于，实施例2的珠光粉体的粒径为30μm-150μm。
实施例3
实施例3与实施例2的区别仅在于，实施例3的珠光粉体的衬底为玻璃衬底。
实施例4
实施例4与实施例1的区别仅在于，实施例4的珠光粉体的覆盖层为氧化铁和二氧化钛，珠光粉体的颜色为金色。
实施例5
实施例5与实施例1的区别仅在于，实施例5的珠光粉体的覆盖层为氧化铁，珠光粉体的颜色为红棕色。
实施例6
实施例6与实施例1的区别仅在于，实施例6的珠光粉体的覆盖层为有机色淀和二氧化钛，珠光粉体的颜色为玫红色。
实施例7
实施例7与实施例1的区别仅在于，实施例7中片状结构的月桂酰赖氨酸粉体的质量为1g。
实施例8
实施例8与实施例1的区别仅在于，实施例8中片状结构的月桂酰赖氨酸粉体的质量为100g。
实施例9
实施例9与实施例1的区别仅在于，实施例9中全氟辛基三乙氧基硅烷的质量为1g。
实施例10
实施例10与实施例1的区别仅在于，实施例10中全氟辛基三乙氧基硅烷的质量为100g。
对比例1
对比例1与实施例1的区别仅在于，对比例1的混合过程中没有加入全氟辛基三乙氧基硅烷。
对比例2
对比例2与实施例1的区别仅在于，对比例2的混合过程中没有加入月 桂酰赖氨酸粉体。
将各实施例的珠光粉体以及各实施例和对比例获得的改性珠光粉体分散于水和白油中，确定分散性，结果如表1所示。
表1
应用实施例1-1
眼影：该眼影包括A相、B相和C相，其中，A相包括云母、滑石粉、硅石、甲基丙烯酸甲酯交联聚合物、肉豆蔻酸镁、硬脂酸镁，B相包括聚二甲基硅氧烷、辛酸/癸酸甘油三酯、异壬酸异壬酯、VP/十六碳烯共聚物，C相为实施例1的改性珠光粉体。以总质量100％计，云母的质量百分数为50％，滑石粉的质量百分数为20％，硅石的质量百分数为5％，甲基丙烯酸甲酯交联聚合物的质量百分数为3％，肉豆蔻酸镁的质量百分数为1％，硬脂酸镁的质量百分数为1％，聚二甲基硅氧烷的质量百分数为3％，辛酸/癸酸甘油三酯的质量百分数为2％，异壬酸异壬酯的质量百分数为2％，VP/十六碳烯共聚物的质量百分数为1％，改性珠光粉体的质量百分数为12％。
制备时，先将A相加入搅拌锅内高速搅拌均匀，然后将B相混合后加入A相中继续以高速搅拌均匀，再将C相加入混合均匀的A相和B相中，低速混合均匀，最后出料、压制成型，得到眼影。
应用实施例1-2～1-6
应用实施例1-2～1-6的组成及其质量百分数参照应用实施例1-1，区别在于C相分别使用实施例2-6的改性珠光粉体。
应用对比例1-1～1-6
应用对比例1-1～1-6的组成及其质量百分数参照应用实施例1-1，区别在于C相分别使用实施例1-6的珠光粉体。
应用对比例1-7～1-8
应用对比例1-7～1-8的组成及其质量百分数参照应用实施例1-1，区别在于C相分别使用对比例1-2的改性珠光粉体。
将该应用实施例1-1和应用对比例1-1获得的眼影涂抹于皮肤上，结果 如图5所示，右侧为应用实施例1-1的眼影的涂抹效果，左侧为应用对比例1-1的眼影的涂抹效果，由图5可知，使用本申请改性珠光粉体的眼影铺展性更好，更贴肤，持妆性更好。
将应用实施例1-1～1-6和应用对比例1-1～1-8的眼影进行光泽度、贴肤柔软度以及持妆性测试，结果如表2所示，其中，1分-10分中，分数高则光泽度高，分数高则柔软贴肤性好，分数高则持妆性好。
表2
应用实施例2-1
液体眼影：该液体眼影包括去离子水、甘油、黄原胶、O/W乳化剂、聚氨酯以及实施例1的改性珠光粉体。以总质量100％计，去离子水的质量百分数为67.5％，甘油的质量百分数为10％，黄原胶的质量百分数为0.5％，O/W乳化剂的质量百分数为1.5％，实施例1的改性珠光粉的质量百分数为20％，聚氨酯的质量百分数为0.5％。
应用实施例2-2～2-6
应用实施例2-2～2-6的组成及其质量百分数参照应用实施例2-1，区别在 于分别使用实施例2-6的改性珠光粉体。
应用对比例2-1～2-6
应用对比例2-1～2-6的组成及其质量百分数参照应用实施例2-1，区别在于分别使用实施例1-6的珠光粉体。
应用对比例2-7～2-8
应用对比例2-7～2-8的组成及其质量百分数参照应用实施例2-1，区别在于分别使用对比例1-2的改性珠光粉体。
将应用实施例2-6和应用对比例1-8的液体眼影进行光泽度、贴肤柔软度以及持妆性测试，结果如表3所示，其中，1分-10分中，分数高则光泽度高，分数高则柔软贴肤性好，分数高则持妆性好。
表3
应用实施例3-1
高光提亮液：该产品包括A相、B相和C相，其中，A相包括聚二甲基硅氧烷、异十二烷、环五聚二甲基硅氧烷、二硬脂二甲铵锂蒙脱石、苯基聚三甲基硅氧烷、PEG-10聚二甲基硅氧烷、辛酸/癸酸甘油三酯、三甲基硅烷 氧基硅酸酯、聚甲基硅倍半氧烷，B相包括水、酒精，C相为实施例1的改性珠光粉体。以总质量100％计，聚二甲基硅氧烷的质量百分数为9％，异十二烷的质量百分数为14.3％，环五聚二甲基硅氧烷的质量百分数为20％，二硬脂二甲铵锂蒙脱石的质量百分数为0.7％，苯基聚三甲基硅氧烷的质量百分数为6％，PEG-10聚二甲基硅氧烷的质量百分数为3％，辛酸/癸酸甘油三酯的质量百分数为5％，三甲基硅烷氧基硅酸酯的质量百分数为2％，聚甲基硅倍半氧烷的质量百分数为5％，水的质量百分数为5％，酒精的质量百分数为12％，改性珠光粉体的质量百分数为18％。
制备时，先将A相加入烧杯，中速搅拌均匀，然后将B相混合后加入A相中均质10分钟，再将C相加入混合均匀的A相和B相中，低速混合均匀，得到高光提亮液。
应用实施例3-2～3-6
应用实施例3-2～3-6的组成及其质量百分数参照应用实施例3-1，区别在于C相分别使用实施例2-6的改性珠光粉体。
应用对比例3-1～3-6
应用对比例3-1～3-6的组成及其质量百分数参照应用实施例3-1，区别在于C相分别使用实施例1-6的珠光粉体。
应用对比例3-7～3-8
应用对比例3-7～3-8的组成及其质量百分数参照应用实施例3-1，区别在于C相分别使用对比例1-2的改性珠光粉体。
将应用实施例3-1～3-6和应用对比例3-1～3-8的高光提亮液进行光泽度、贴肤柔软度以及持妆性测试，结果如表4所示，其中，1分-10分中，分数高则光泽度高，分数高则柔软贴肤性好，分数高则持妆性好。
表4
应用实施例4-1
高光提亮液(W/O型)：该乳化型产品包括A相、B相、C相和D相，其中，A相包括PEG-10聚二甲基硅氧烷、月桂基PEG-9聚二甲基硅氧乙基聚二甲基硅氧烷、苯基聚三甲基硅氧烷、辛酸\癸酸甘油三酯、辛基十二醇、丁二醇二辛酸/二癸酸酯、三甲基硅烷氧基硅酸酯和/或聚二甲基硅氧烷、C9-12烷，B相包括环五聚二甲基硅氧烷、二硬脂二甲铵锂蒙脱石，C相包括水、甘油、硫酸镁、丙二醇、苯氧乙醇/乙基己基甘油，D相为实施例1的改性珠光粉体。以总质量100％计，PEG-10聚二甲基硅氧烷的质量百分数为2％，月桂基PEG-9聚二甲基硅氧乙基聚二甲基硅氧烷的质量百分数为1％，苯基聚三甲基硅氧烷的质量百分数为7％，辛酸\癸酸甘油三酯的质量百分数为4％，辛基十二醇的质量百分数为5％，丁二醇二辛酸/二癸酸酯的质量百分数为5％，三甲基硅烷氧基硅酸酯的质量百分数为2％，C9-12烷的质量百分数为6％，环五聚二甲基硅氧烷的质量百分数为15％，二硬脂二甲铵锂蒙脱石的质量百分数为1％，水的质量百分数为30.55％，甘油的质量百分数为 5％，硫酸镁的质量百分数为0.7％，丙二醇的质量百分数为5％，苯氧乙醇/乙基己基甘油的质量百分数为0.75％，改性珠光粉体的质量百分数为10％。
制备时，先将A相加入烧杯，60℃搅拌分散均匀，然后将B相混合后加入A相中均质5分钟，然后边均质边加入C相，加完C相后再均质5分钟，再将D相加入混合均匀的A相、B相和C相中，低速混合均匀，得到高光提亮液(W/O型)。
应用实施例4-2～4-6
应用实施例4-2～4-6的组成及其质量百分数参照应用实施例4-1，区别在于D相分别使用实施例2-6的改性珠光粉体。
应用对比例4-1～4-6
应用对比例4-1～4-6的组成及其质量百分数参照应用实施例4-1，区别在于D相分别使用实施例1-6的珠光粉体。
应用对比例4-7～4-8
应用对比例4-7～4-8的组成及其质量百分数参照应用实施例3-1，区别在于C相分别使用对比例1-2的改性珠光粉体。
将应用实施例4-1～4-6和应用对比例4-1～4-8的高光提亮液(W/O型)进行光泽度、贴肤柔软度以及持妆性测试，结果如表5所示，其中，1分-10分中，分数高则光泽度高，分数高则柔软贴肤性好，分数高则持妆性好。
表5
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本申请的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本申请构思的前提下，还可以做出若干变形和改进，这些都属于本申请的保护范围。因此，本申请专利的保护范围应以所附权利要求为准。
Claims (10)
- 一种改性珠光粉体，其特征在于，所述改性珠光粉体包括珠光粉体、覆盖于所述珠光粉体表面的月桂酰赖氨酸粉体以及通过共价键连接于所述珠光粉体的含氟硅烷偶联剂。
- 根据权利要求1所述的改性珠光粉体，其中，所述月桂酰赖氨酸粉体为片状结构。
- 根据权利要求1所述的改性珠光粉体，其中，部分所述含氟硅烷偶联剂相互缔和形成网状结构。
- 根据权利要求1所述的改性珠光粉体，其中，所述含氟硅烷偶联剂的质量为所述珠光粉体的质量的0.1％-10.0％，所述月桂酰赖氨酸粉体的质量为所述珠光粉体的质量的0.1％-10.0％。
- 根据权利要求1所述的改性珠光粉体，其中，所述含氟硅烷偶联剂的通式为R-Si-(OC mH 2m+1) 3，式中，R为C nF 2n+1-(CH 2) 2-，1≤n≤6，n为整数，m为1或2。
- 根据权利要求5所述的改性珠光粉体，其中，所述含氟硅烷偶联剂包括全氟辛基三乙氧基硅烷、十三氟辛基三甲氧基硅烷、十七氟癸基三甲氧基硅烷中的至少一种。
- 一种如权利要求1-6任一项所述改性珠光粉体的制备方法，其特征在于，包括：将珠光粉体、含氟硅烷偶联剂以及月桂酰赖氨酸粉体混合，加热，得到改性珠光粉体。
- 根据权利要求7所述的改性珠光粉体的制备方法，其中，所述加热的温度为100℃-120℃，时间为1小时-3小时。
- 一种化妆品，其特征在于，所述化妆品包括如权利要求1-6任一项所 述的改性珠光粉体。
- 根据权利要求9所述的化妆品，其中，所述改性珠光粉体于所述化妆品中定向分布。
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