CN114366686B - Surface treatment powder and preparation method and application thereof - Google Patents

Surface treatment powder and preparation method and application thereof Download PDF

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CN114366686B
CN114366686B CN202111509512.7A CN202111509512A CN114366686B CN 114366686 B CN114366686 B CN 114366686B CN 202111509512 A CN202111509512 A CN 202111509512A CN 114366686 B CN114366686 B CN 114366686B
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powder
prebiotics
surface treatment
oligosaccharide
mass
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CN114366686A (en
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陈宗乐
吴建军
张文彬
刘晗
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Shanghai Co Fun Biotech Co ltd
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Shanghai Co Fun Biotech Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/23Sulfur; Selenium; Tellurium; Compounds thereof
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    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
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    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
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    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
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    • A61K8/39Derivatives containing from 2 to 10 oxyalkylene groups
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    • A61K8/98Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin
    • A61K8/987Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution of animal origin of species other than mammals or birds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
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    • AHUMAN NECESSITIES
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    • A61Q19/00Preparations for care of the skin
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    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/60Particulates further characterized by their structure or composition
    • A61K2800/61Surface treated
    • A61K2800/612By organic compounds
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
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Abstract

The invention relates to surface treatment powder, which comprises base powder, and prebiotics and glycerol polymers attached to the base powder, wherein the mass of the prebiotics is 0.1-8% of the mass of the surface treatment powder. The invention also relates to a preparation method of the surface treatment powder and application of the surface treatment powder in water-based cosmetics. The surface treatment powder has excellent hydrophilicity and dispersibility, and the aqueous cosmetic using the surface treatment powder has super-strong stability and is not easy to settle and delaminate after being placed for a long time.

Description

Surface treatment powder and preparation method and application thereof
Technical Field
The invention relates to the technical field of cosmetics, in particular to surface treatment powder and a preparation method and application thereof.
Background
The traditional organic surface treatment modes of the powder for the cosmetics are as follows: organosilicon surface treatment, fluorine-containing surface treatment, titanate coupling agent surface treatment, organic acid and salt surface treatment, amino acid surface treatment and composite surface treatment formed by any two or more treatment types.
The organosilicon surface treatment is to combine organosilicon molecules on the surface of the powder by chemical bonds, so that the powder has excellent hydrophobicity, ductility, fluidity, dispersibility and adsorptivity, and is suitable for cosmetics of silicone oil systems. The fluorine-containing surface treatment is based on the organosilicon surface treatment, and the effect of the surface treatment is further improved through the synergistic effect of fluorine-containing groups. The titanate coupling agent surface treatment is to make the surface of the powder form a layer of uniform isostearate group film by chemical bonding of alkoxy groups and hydroxyl groups on the surface of the powder, and has excellent lipophilicity, skin adhesion and hydrophobicity. The surface treatment of the organic acid and the salt thereof can change the charge of the surface of the powder, and the surface treatment of the amino acid can introduce specific active groups, so that the powder has more excellent skin-friendly effect.
Although these surface treatments can improve the effect of the powder in terms of hydrophobicity, oleophobicity, skin feel, etc., when these surface-treated powders are used in aqueous cosmetics, problems such as sedimentation and delamination are still likely to occur, and long-term stability is poor.
Disclosure of Invention
Based on this, it is necessary to provide a surface-treated powder, a method for producing the same and an application thereof, in view of the above-mentioned problems; the surface treatment powder has excellent hydrophilicity and dispersibility, and the aqueous cosmetic using the surface treatment powder has super-strong stability and is not easy to settle and agglomerate after long-term placement.
A surface-treated powder comprising a base powder, and a prebiotic and a glycerol polymer attached to the base powder, the glycerol polymer being selected from glycerol polymers, wherein the mass of the prebiotic is 0.1% -8% of the mass of the surface-treated powder.
In one embodiment, the mass of the glycerol polymer is 0.1% -15% of the mass of the surface-treated powder.
In one embodiment, the prebiotic comprises at least one of fructo-oligosaccharide, galacto-oligosaccharide, fructo-oligosaccharide, soy-oligosaccharide, galacto-oligosaccharide, isomalto-oligosaccharide, xylo-oligosaccharide, mannooligosaccharide, chitosan oligosaccharide, lactitol, isomaltulose, soy-oligosaccharide, xylo-oligosaccharide, and malto-oligosaccharide.
In one embodiment, the glycerol polymer comprises at least one of polyglycerol-4, polyglycerol-6, polyglycerol-8, and polyglycerol-10.
In one embodiment, the base powder comprises at least one of micro-sized titanium dioxide, nano-sized zinc oxide, iron oxide yellow, iron oxide red, iron oxide black, chromium oxide green, ultramarine, talc, mica, pearlescence, kaolin, barium sulfate, calcium sulfate hydrate, pearl powder, perlite, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, calcium carbonate, magnesium carbonate, calcium pyrophosphate, and calcium phosphate.
In the surface treatment powder, the glycerol polymer can provide rich polar hydroxyl groups to form stronger hydrogen bond, so that the prebiotics and the glycerol polymer can be firmly and uniformly coated on the surface of the base powder, and the surface treatment powder has good hydrophilic performance. Meanwhile, the coating layer formed by the prebiotics and the glycerol polymer can provide a good steric hindrance effect for the coated basic powder, so that the surface treatment powder has excellent dispersibility and super-strong stability, is not easy to agglomerate, and can be better applied to the aqueous cosmetics.
The preparation method of the surface treatment powder comprises the following steps:
mixing the prebiotics with water to obtain an aqueous solution of the prebiotics;
mixing a glycerol polymer with the aqueous solution of the prebiotics to obtain a mixed treatment solution;
and spraying the mixed treatment liquid on the basic powder under the condition of stirring, and drying and crushing to obtain the surface treatment powder.
In one embodiment, the prebiotic has a mass of 0.1% to 100% of the mass of water.
In one embodiment, the mass of the prebiotic is 0.1% -10% of the mass of the base powder.
In one embodiment, the mass of the glycerol polymer is 0.1% -20% of the mass of the base powder.
In the preparation method of the surface treatment powder, the prebiotics which are solid at normal temperature are dissolved and then are used for wetting the base powder, and in the drying process, the dissolved prebiotics can be recrystallized and deposited on the surface of the base powder, so that the coating of the prebiotics is firmer, and the coating utilization rate is up to more than 90%. And the prebiotics and the glycerol polymer are respectively completely dissolved, and then the basic powder is coated, so that the prebiotics and the glycerol polymer are more firmly coated, and the problem that a large number of agglomerated hard particles are generated due to incomplete dissolution of the prebiotics and higher viscosity of the glycerol polymer in the coating process can be avoided, thereby effectively improving the coating quality and being beneficial to obtaining the surface treatment powder which is uniformly coated by the prebiotics and the glycerol polymer and is hydrophilic and easy to disperse.
The application of the surface treatment powder in the water-based cosmetics.
The surface treatment powder can be widely used as a raw material in aqueous cosmetics, so that the aqueous cosmetics have super-strong stability, are not easy to settle and delaminate after being placed for a long time, have good compatibility with other components, and are favorable for carrying out formula design on the cosmetics so as to obtain cosmetics with stable quality, improved skin microecology and excellent safety on organisms and environment.
Drawings
FIG. 1 is a scanning electron microscope image of the surface-treated powder prepared in example 1;
fig. 2 is a comparative image of the dispersibility effect in water of the surface-treated powder prepared in example 1 and the surface-treated powder prepared in comparative example 1.
Detailed Description
The surface-treated powder, the method for preparing the same and the use thereof according to the present invention will be further described below.
The surface treatment powder provided by the invention comprises basic powder, and prebiotics and glycerol polymers attached to the basic powder, wherein the mass of the prebiotics is 0.1% -8% of the mass of the surface treatment powder.
In the surface treatment powder, the glycerol polymer can provide rich polar hydroxyl groups, so that a strong hydrogen bond effect is formed, the prebiotics and the glycerol polymer can be firmly and uniformly coated on the surface of the base powder, the hydrophilic effect of the surface treatment powder is further enhanced, and the dispersibility is improved.
Meanwhile, the coating layer formed by the prebiotics and the glycerol polymer can provide a good steric hindrance effect for the coated basic powder, so that the surface treatment powder has excellent dispersibility and super-strong stability, is not easy to agglomerate, and can be better applied to the aqueous cosmetics.
In order to ensure the coating effect of the prebiotics, the mass of the prebiotics is preferably 0.1% -5% of the surface treatment powder. The mass of the glycerol polymer is 0.1% -15% of the mass of the surface treatment powder, preferably 5% -15%.
Optionally, the prebiotic comprises at least one of fructo-oligosaccharide, galacto-oligosaccharide, fructo-oligosaccharide, soy-oligosaccharide, galacto-oligosaccharide, isomalto-oligosaccharide, xylo-oligosaccharide, mannooligosaccharide, chitosan oligosaccharide, lactitol, isomaltulose, soy-oligosaccharide, xylo-oligosaccharide, and malto-oligosaccharide; the glycerol polymer comprises at least one of polyglycerol-4, polyglycerol-6, polyglycerol-8 and polyglycerol-10.
Optionally, the basic powder comprises at least one of micron-sized titanium dioxide, nanoscale zinc oxide, iron oxide yellow, iron oxide red, iron oxide black, chromium oxide green, ultramarine, talcum, mica, pearlescence, kaolin, barium sulfate, calcium sulfate hydrate, pearl powder, perlite, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, calcium carbonate, magnesium carbonate, calcium pyrophosphate and calcium phosphate. Wherein the mica is at least one selected from sericite, synthetic fluorophlogopite and crystal mica, the zinc carbonate is basic zinc carbonate, and the magnesium carbonate is basic magnesium carbonate.
The invention also provides a preparation method of the surface treatment powder, which comprises the following steps:
s1, mixing prebiotics with water to obtain an aqueous solution of the prebiotics;
s2, mixing a glycerol polymer with the aqueous solution of the prebiotics to obtain a mixed treatment solution;
and S3, spraying the mixed treatment liquid on the basic powder under the condition of stirring, and drying and crushing to obtain the surface treatment powder.
Because the prebiotics are solid at normal temperature and have poor solubility in the glycerol polymer, if the prebiotics are directly mixed with the glycerol polymer, the prebiotics are incompletely dissolved due to higher viscosity of the glycerol polymer, so that the prebiotics are coated unevenly and a large number of hard particles are produced, the coating quality of the surface treatment powder is poor, and meanwhile, the coating utilization rate of the prebiotics is low, and the problems of raw material waste and the like exist.
In addition, although the glycerol polymer can provide rich polar hydroxyl groups, the adsorption of the glycerol polymer and the prebiotics on the surface of the basic powder is effectively enhanced, the glycerol polymer has certain viscosity, so that the glycerol polymer is unevenly coated, and even the basic powder is agglomerated.
Therefore, in the invention, in the step S1, the prebiotics are mixed with water and completely dissolved to form an aqueous solution of the prebiotics, and then in the step S2, the glycerol polymer is mixed with the aqueous solution of the prebiotics to obtain the mixed treatment liquid. The steps S1-S2 can avoid the problem that a large number of agglomerated hard particles are generated due to incomplete dissolution of prebiotics and higher viscosity of the glycerol polymer in the coating process, thereby effectively improving the coating quality and being beneficial to obtaining the surface treatment powder which is uniformly coated by the prebiotics and the glycerol polymer and is hydrophilic and easy to disperse; meanwhile, the coating utilization rate of the prebiotics is improved.
In an embodiment, in order to ensure complete dissolution of the prebiotics, while achieving a certain coating amount of the prebiotics, the mass of the prebiotics is 0.1-100%, preferably 0.1-50% of the mass of the water; the mass of the prebiotics is 0.1-10% of the mass of the basic powder, preferably 0.1-9%.
In order to coordinate the dosage of the glycerol polymer and the prebiotics and ensure that the viscosity of the mixed treatment fluid is proper, the mass of the glycerol polymer is 0.1-20 percent, preferably 5-15 percent of the mass of the base powder.
In the step S3, the dissolved prebiotics can be recrystallized and deposited on the surface of the basic powder through the drying process, compared with the coating effect by means of intermolecular acting force, the coating mode of the invention ensures that the prebiotics are coated more firmly and are not easy to fall off, the coating utilization rate of the prebiotics is up to more than 90%, the coating effect of 100% can be basically realized, the utilization rate of raw materials is effectively improved, and the raw material waste is reduced.
Optionally, the temperature of drying the base powder after mixing and stirring with the mixed treatment liquid is 100-130 ℃, preferably 105-120 ℃ and the time is 0.5-4 h, preferably 1-3 h.
The invention also provides application of the surface treatment powder in the water-based cosmetics.
The surface treatment powder can be widely used as a raw material in aqueous cosmetics, so that the aqueous cosmetics have super-strong stability, are not easy to settle and delaminate after being placed for a long time, have good compatibility with other components, and are favorable for carrying out formula design on the cosmetics so as to obtain cosmetics with stable quality, improved skin microecology and excellent safety on organisms and environment.
Hereinafter, the surface-treated powder, and the preparation method and application thereof will be further described by way of the following specific examples.
Example 1
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of polyglycerol-4 and an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution onto 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder shown in figure 1.
Example 2
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of polyglycerol-6 and an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of iron oxide yellow under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Example 3
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of polyglycerol-10 and an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of iron oxide red under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Example 4
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of polyglycerol-10 and an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of iron oxide black under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Example 5
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of polyglycerol-6 and an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of nano zinc oxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Example 6
Uniformly mixing 2g of galacto-oligosaccharide with 5g of water to obtain an aqueous solution of lactulose; uniformly mixing 5g of polyglycerol-4 and an aqueous solution of lactulose to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Example 7
Example 7 differs from example 1 only in that the base powder of example 7 is mica.
Example 8
Example 8 differs from example 1 only in that the base powder of example 8 is a pearl powder.
Example 9
Example 9 differs from example 1 only in that the base powder of example 9 is zinc carbonate.
Example 10
Example 10 differs from example 1 only in that the base powder of example 10 is calcium carbonate.
Example 11
Example 11 differs from example 1 only in that the fructooligosaccharide of example 11 is 0.5g.
Example 12
Example 12 differs from example 1 only in that the fructooligosaccharides of example 12 are 3.5g.
Example 13
Example 13 differs from example 1 only in that the fructooligosaccharides of example 13 are 5g.
Example 14
Example 14 differs from example 1 only in that the fructooligosaccharides of example 14 are 6.5g.
Example 15
Example 15 differs from example 1 only in that the fructooligosaccharides of example 15 are 8g.
Comparative example 1
Directly mixing 2g of fructo-oligosaccharide, 5g of water and 5g of polyglycerol-4 to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Comparative example 2
Directly mixing 2g of fructo-oligosaccharide with 5g of polyglycerol-4 to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Comparative example 3
Uniformly mixing 2g of D-panthenol with 5g of water to obtain an aqueous solution of D-panthenol; uniformly mixing 5g of polyglycerol-4 and an aqueous solution of D-panthenol to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Comparative example 4
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of glycerol with an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Comparative example 5
Uniformly mixing 2g of fructo-oligosaccharide with 5g of water to obtain an aqueous solution of fructo-oligosaccharide; uniformly mixing 5g of PEG-8 with an aqueous solution of fructo-oligosaccharide to obtain a mixed treatment solution; spraying the mixed treatment solution on 100g of micron-sized titanium dioxide under the condition of stirring, uniformly stirring, transferring to a drying oven, drying at 120 ℃ for 2 hours, and carrying out jet milling to obtain the surface treatment powder.
Test the coating effect of examples 1-15, test method: the surface-treated powder was heated by mixing with a strong acid and evaluated using resorcinol. The results were all red, indicating that the fructooligosaccharides were successfully coated on the base powder.
Examples 1-15 were subjected to a coating fastness test, test method: mixing and stirring the surface treatment powder and water for 1h under the water bath condition of 80 ℃, filtering, and identifying the filtered powder by using resorcinol, wherein the result shows that the product is red and has consistent color, and the surface of the surface treatment powder still has a large amount of fructo-oligosaccharides after a strict washing process, which indicates that the coating firmness of the fructo-oligosaccharides is good.
The coating availability of the prebiotics and D-panthenol in the surface treated powders obtained in examples 1 to 15, the powders obtained in comparative examples 1 to 5 are shown in Table 1.
TABLE 1
As can be seen from Table 1, the coating availability of the moisturizing component in the lipophilic dispersion powders coated with the moisturizing component obtained in examples 1 to 15 is over 90%, while the coating availability of comparative examples 1 to 5 is only up to 51.2%, so that the preparation method provided by the invention can achieve the coating availability of the moisturizing component as high as over 90%.
The particle size distribution of the surface-treated powders obtained in examples 1 to 15 and the powders obtained in comparative examples 1 to 5 was measured, and the results are shown in Table 2.
TABLE 2
As can be seen from FIGS. 1 and 2, the surface-treated powders obtained in examples 1 to 15 of the present invention were uniform in size distribution, whereas the powders obtained in comparative examples 1 to 5 produced hard particles due to agglomeration and agglomeration, and the large particles having large differences in size distribution, showing that the surface-treated powders prepared by the present invention were uniform in particles, good in dispersibility, and free from agglomeration.
The water absorption value of the base powders of examples 1 to 15, comparative examples 1 to 5, the surface-treated powders obtained, and the surface-treated powders after washing treatment were tested, and the results are shown in Table 3. Washing: mixing the surface treatment powder with water under the water bath condition of 80 ℃ and stirring for 1h, and then filtering and drying.
TABLE 3 Table 3
As is clear from table 3, the surface-treated powders obtained in examples 1 to 15 of the present invention were excellent in water absorption effect, and the water absorption effect before washing was maintained after the washing treatment, which also proves that the prebiotic coating fastness of the surface-treated powders of the present invention was good.
The surface-treated powder obtained in example 1 and the surface-treated powder obtained in comparative example 1 were subjected to a dispersibility test, and the test results were recorded in table 4. The testing method comprises the following steps: the surface-treated powder obtained in example 1 and the surface-treated powder obtained in comparative example 1 were each prepared as a 1% aqueous dispersion, and after simultaneous shaking and dispersion, they were allowed to stand for 30 minutes, and the sedimentation of the particles of the surface-treated powder at the bottom was observed, and as a result, as shown in fig. 2, a is a graph showing the effect of dispersion of the 1% aqueous dispersion of the surface-treated powder obtained in example 1 after standing and inverted, and B is a graph showing the effect of dispersion of the 1% aqueous dispersion of the surface-treated powder obtained in comparative example 1 after standing and inverted, as is clear from fig. 2, the effect of dispersion was excellent with little powder sedimentation at the bottom of the 1% aqueous dispersion of the surface-treated powder obtained in comparative example 1, whereas the effect of dispersion was poor with a large amount of powder sedimentation at the bottom of the 1% aqueous dispersion of the surface-treated powder obtained in comparative example 1.
The surface-treated powders obtained in examples 2 to 15 and the powders obtained in comparative examples 2 to 4 were subjected to dispersibility test, and the results are shown in Table 4.
TABLE 4 Table 4
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As is clear from Table 4, the surface-treated powders obtained in examples 1 to 15 of the present invention were self-dispersible in both water and propylene glycol and had no agglomerated particles, whereas the powders obtained in comparative examples 1 to 5 were poor in dispersion effect and were liable to generate agglomerated particles. Therefore, the surface-treated powder obtained by the present invention has excellent dispersibility.
Application example 1
The surface-treated powders obtained in examples 1 and 6 of the present invention and the surface-treated powders obtained in comparative examples 1 and 3 were formulated in accordance with the formulations shown in Table 5, to obtain foundation liquid samples a to d.
The preparation process comprises the following steps: mixing and stirring the phase A, and heating to 75 ℃ for standby; stirring phase C uniformly, and heating to 75 ℃; adding the powder of the phase B into the phase C, stirring and dispersing uniformly, and homogenizing for 30 seconds; slowly adding the phase A into the phase BC under rapid stirring, and homogenizing for 1 minute after the emulsification is completed; adding the phase D into the phase ABC under rapid stirring, uniformly stirring, and homogenizing for 1 minute; cooling to below 45deg.C, adding phase E, stirring, and discharging to obtain powder base solution.
TABLE 5
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Carrying out stability test on the prepared foundation liquid samples a-d, wherein the test method comprises the following steps of: freeze thawing cycle test (one cycle including high temperature-8+ -2deg.C, 24h and low temperature 40+ -1deg.C, 24 h) and normal temperature stability test (15-25deg.C). The test results are shown in Table 6.
TABLE 6
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As can be seen from table 6, the foundation liquid samples a and b obtained by the surface treatment powder preparation obtained in examples 1 and 6 of the present invention still show a uniform dispersion effect after the freeze thawing cycle and the normal temperature test for three months, and no sedimentation and delamination phenomenon, while the foundation liquid samples c and d obtained by the surface treatment powder preparation obtained in comparative examples 1 and 3 start to sediment after the second time of the freeze thawing cycle and the second month of the normal temperature test, respectively, and generate obvious delamination after the third time of the freeze thawing cycle and the third month of the normal temperature test. Therefore, the surface-treated powders obtained in examples 1 and 6 of the present invention were prepared to give a foundation liquid having superior stability.
Application example 2
The surface-treated powders obtained in examples 1 and 6 of the present invention and the powders obtained in comparative examples 1 and 3 were formulated according to the formulations shown in Table 7 to obtain toner water samples a to d.
The preparation process comprises the following steps: mixing and stirring the phase A, and heating to 75 ℃ for standby; stirring phase C uniformly, and heating to 75 ℃; adding the powder of the phase B into the phase C, stirring and dispersing uniformly, and homogenizing for 30 seconds; slowly adding the phase A into the phase BC under rapid stirring, and homogenizing for 1 minute after the emulsification is completed; adding the phase D into the phase ABC under rapid stirring, uniformly stirring, and homogenizing for 1 minute; cooling to below 45 ℃, adding the E phase, stirring and discharging to obtain the toner.
TABLE 7
The stability test is carried out on the prepared toner water samples a-d, and the test method comprises the following steps: freeze thawing cycle test (one cycle including high temperature-8+ -2deg.C, 24h and low temperature 40+ -1deg.C, 24 h) and normal temperature stability test (15-25deg.C). The test results are shown in Table 8.
TABLE 8
As can be seen from table 8, the toner water samples a and b obtained by the surface treatment powder preparation obtained in examples 1 and 6 of the present invention still show a uniformly dispersed effect after the freeze thawing cycle and the normal temperature test for three months, and no sedimentation and delamination phenomenon, while the toner water samples c and d obtained by the surface treatment powder preparation obtained in comparative examples 1 and 3 start to sediment after the second time of the freeze thawing cycle and the second month of the normal temperature test, respectively, and generate obvious delamination after the third time of the freeze thawing cycle and the third month of the normal temperature test. Therefore, the toner prepared from the surface treatment powder obtained in examples 1 and 6 of the present invention has superior stability.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (4)

1. The surface treatment powder is characterized by comprising a base powder, and prebiotics and glycerol polymers attached to the base powder, wherein the mass of the prebiotics is 0.1-8% of the mass of the surface treatment powder, and the mass of the glycerol polymers is 0.1-15% of the mass of the surface treatment powder;
the prebiotics are at least one of fructo-oligosaccharide, soybean oligosaccharide, galacto-oligosaccharide, isomalto-oligosaccharide, xylo-oligosaccharide, mannooligosaccharide, chitosan oligosaccharide, isomaltulose and isomaltooligosaccharide;
the glycerol polymer is at least one of polyglycerol-4, polyglycerol-6, polyglycerol-8 and polyglycerol-10;
the basic powder is at least one of micron-sized titanium dioxide, nanoscale zinc oxide, iron oxide yellow, iron oxide red, iron oxide black, chromium oxide green, ultramarine, talcum, mica, kaolin, barium sulfate, calcium sulfate hydrate, pearl powder, magnesium sulfate, aluminum sulfate, bismuth oxychloride, zinc carbonate, calcium carbonate, magnesium carbonate, calcium pyrophosphate and calcium phosphate;
the preparation method of the surface treatment powder comprises the following steps:
mixing the prebiotics with water to obtain an aqueous solution of the prebiotics;
mixing a glycerol polymer with the aqueous solution of the prebiotics to obtain a mixed treatment solution; and
and spraying the mixed treatment liquid on the basic powder under the condition of stirring, and drying and crushing to obtain the surface treatment powder.
2. A method for preparing the surface-treated powder according to claim 1, comprising the steps of:
mixing the prebiotics with water to obtain an aqueous solution of the prebiotics;
mixing a glycerol polymer with the aqueous solution of the prebiotics to obtain a mixed treatment solution; and
and spraying the mixed treatment liquid on the basic powder under the condition of stirring, and drying and crushing to obtain the surface treatment powder.
3. The method of preparing a surface-treated powder according to claim 2, wherein the mass of the prebiotic is 0.1% -100% of the mass of the water.
4. Use of the surface-treated powder according to claim 1 in an aqueous cosmetic.
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