CN117731546A - Azelaic acid-silica composite powder as well as preparation method and application thereof - Google Patents
Azelaic acid-silica composite powder as well as preparation method and application thereof Download PDFInfo
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- CN117731546A CN117731546A CN202311753813.3A CN202311753813A CN117731546A CN 117731546 A CN117731546 A CN 117731546A CN 202311753813 A CN202311753813 A CN 202311753813A CN 117731546 A CN117731546 A CN 117731546A
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- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 title claims abstract description 451
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 245
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 153
- 239000000843 powder Substances 0.000 title claims abstract description 79
- 239000002131 composite material Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 45
- 238000001035 drying Methods 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000002245 particle Substances 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000011282 treatment Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
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- 239000002585 base Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
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- 208000002874 Acne Vulgaris Diseases 0.000 description 2
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- 206010000496 acne Diseases 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
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- 150000003839 salts Chemical class 0.000 description 2
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- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to azelaic acid-silica composite powder as well as a preparation method and application thereof. The preparation method comprises the following steps: mixing azelaic acid with a solvent to obtain an azelaic acid solution, wherein the mass ratio of the azelaic acid to the solvent is 1:1-1:8; mixing the azelaic acid solution with silica to obtain a mixture; and drying the mixture to obtain azelaic acid-silica composite powder, wherein the drying temperature is 10-80 ℃ higher than the volatilization temperature of the solvent. According to the invention, effective recombination of azelaic acid and silica is realized by recrystallization, azelaic acid is uniformly loaded on the surface of the silica, the utilization rate of azelaic acid is effectively improved, the problems of heavy granular feel and poor skin feel of azelaic acid are solved, in addition, the surface acid-base number of the prepared azelaic acid-silica composite powder is closer to the acid-base environment of the skin, and the azelaic acid-silica composite powder does not contain solvents or other substance additives, so that the irritation to the skin is reduced, and the application field of azelaic acid is greatly widened.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to azelaic acid-silica composite powder as well as a preparation method and application thereof.
Background
In recent years, because of the importance of functional skin care and skin care products, the attention of azelaic acid is continuously rising, and azelaic acid becomes an important component for demarcating skin care components, and has high value in the field of skin care. Azelaic acid can gently remove cutin, effectively avoid pore blockage, improve secretion of skin grease to achieve the effect of controlling oil, inhibit generation and action of anaerobic bacteria, aerobic bacteria and active oxygen free radicals on the surface of skin and in hair follicles, and achieve the effects of resisting bacteria and inflammation. At the same time, azelaic acid is also indicated for long-term maintenance of the vaccinia muscle because it is substantially free of resistance.
However, azelaic acid has extremely low solubility and concentration which is difficult to raise, so that the actual use effect is not ideal; at the same time, azelaic acid is usually present in the form of crystalline powder, a gritty feel is evident, and azelaic acid itself presents acidity, is strongly irritating, and if the problem of solubility of azelaic acid in solvents cannot be solved, increasing its content blindly leads to a rough texture of the product and to irritation of the skin. In addition, azelaic acid has high melting point and poor compatibility, so that the use effect is affected when azelaic acid products exist in low concentration; and when the concentration is high, the oil feel is heavy, the air permeability is poor, the irritation is strong, the user experience is affected, and the like.
In the prior art, azelaic acid and alkali are compounded to form salt azelaic acid generally, so that the solubility of azelaic acid in water is increased, but the original structure of azelaic acid is damaged by alkalization, the use effect is greatly reduced, and the salt azelaic acid is insoluble in grease, so that the application of azelaic acid in the field of color cosmetics, especially in the color cosmetics without alcohol, is severely limited due to the limited selection and collocation of solvents in a formula.
Disclosure of Invention
Based on this, it is necessary to provide an azelaic acid-silica composite powder, a preparation method and application thereof, wherein the azelaic acid-silica composite powder prepared by the preparation method has good skin feel and small skin irritation, and greatly widens the application field of azelaic acid.
The preparation process of azelaic acid-silica composite powder includes the following steps:
mixing azelaic acid with a solvent to obtain an azelaic acid solution, wherein the mass ratio of the azelaic acid to the solvent is 1:1-1:8;
mixing the azelaic acid solution with silica to obtain a mixture;
and drying the mixture to obtain azelaic acid-silica composite powder, wherein the drying temperature is 10-80 ℃ higher than the volatilization temperature of the solvent.
In one embodiment, the mass ratio of azelaic acid to silica is from 3:100 to 3:20.
In one embodiment, the specific surface area of the silica is greater than or equal to 100m 2 /g。
In one embodiment, the silica has a pH of 4.0 to 8.0.
In one embodiment, the azelaic acid solution is mixed with the silica in a manner selected from stirring treatments at a rotational speed of 1000r/min to 25000r/min.
In one embodiment, the solvent is selected from at least one of hot water, an alcohol solvent or a water-alcohol mixture at a temperature of 50 ℃ to 90 ℃.
In one embodiment, the drying temperature is 80-150 ℃ and the drying time is 1-6 h.
An azelaic acid-silica composite powder prepared by the process for preparing an azelaic acid-silica composite powder as described above, which comprises silica and azelaic acid attached to the surface of the silica.
In one embodiment, the particle size ratio of azelaic acid to silica is from 1:10 to 1:3.
Use of the azelaic acid-silica composite powder as described above in a make-up product.
According to the preparation method disclosed by the invention, the effective recombination of the azelaic acid and the silica is realized by utilizing recrystallization, so that the azelaic acid is uniformly loaded on the surface of the silica, the utilization rate of the azelaic acid is effectively improved, the effective contact between the azelaic acid and the skin is obviously increased, so that the effects are better exerted, the problems of granular feel and the like of the azelaic acid are solved, in addition, the prepared azelaic acid-silica composite powder material has a surface acid-base number closer to the acid-base environment of the skin, and does not contain solvents or other material additives, so that the irritation to the skin is reduced, and the application field of the azelaic acid is greatly widened.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required to be used in the embodiments or the description of the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments described in the present invention, and other drawings may be obtained according to the drawings without inventive effort to those skilled in the art.
Figure 1 is an image of blank 1 under a 100-fold oil microscope.
Figure 2 is an image of blank 2 under a 100-fold oil microscope.
Fig. 3 is a scanning electron microscope image of a blank 2, in which the scale length of fig. 3 (a) is 5 μm and the scale length of fig. 3 (b) is 100 μm.
FIG. 4 is a scanning electron microscope image of azelaic acid-silica composite powder prepared in example 2, wherein the scale length of FIG. 4 (a) is 5 μm and the scale length of FIG. 4 (b) is 100. Mu.m.
Detailed Description
The present invention will be described in more detail below in order to facilitate understanding of the present invention. It should be understood, however, that the invention may be embodied in many different forms and is not limited to the implementations or embodiments described herein. Rather, these embodiments or examples are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments or examples only and is not intended to be limiting of the invention. As used herein, the optional scope of the term "and/or" includes any one of the two or more related listed items, as well as any and all combinations of related listed items, including any two or more of the related listed items, or all combinations of related listed items.
The preparation method of azelaic acid-silica composite powder provided by the invention comprises the following steps:
s1, mixing azelaic acid and a solvent to obtain an azelaic acid solution, wherein the mass ratio of the azelaic acid to the solvent is 1:1-1:8;
s2, mixing the azelaic acid solution with silica to obtain a mixture;
s3, drying the mixture to obtain azelaic acid-silica composite powder, wherein the drying temperature is 10-80 ℃ higher than the volatilization temperature of the solvent.
In the step S1, the azelaic acid which is solid at normal temperature is dissolved into liquid state by selecting a proper solvent according to a specific proportion, so that the azelaic acid solution has higher dissolution degree, the subsequent recrystallisation of azelaic acid is facilitated, the problem of massive agglomeration of hard particles of azelaic acid is effectively solved, and the loading effect of azelaic acid is improved.
In one embodiment, the mass ratio of the azelaic acid to the solvent is preferably 1:4-1:6, which is favorable for further promoting the dissolution of the azelaic acid and realizing better dissolution effect.
In one embodiment, the solvent is selected from at least one of hot water, an alcohol solvent or a mixture of water and alcohol at a temperature of 50 to 90 ℃.
In step S2, silica is mixed with the azelaic acid solution, so that the azelaic acid and the silica can be fully combined due to the fact that the silica can provide more landing sites for the azelaic acid, and the good loading of the azelaic acid is facilitated.
In one embodiment, the mass ratio of azelaic acid to silica in the mixture is from 3:100 to 3:20, preferably from 1:20 to 1:12.5, which is advantageous for further enhancing the loading effect of azelaic acid on the silica surface.
In one embodiment, the silica has a specific surface area of 100m or more 2 /g, utensilThe silica with larger specific surface area can provide more landing sites for the azelaic acid, and is more beneficial to improving the loading effect of the azelaic acid on the surface of the silica.
In one embodiment, the pH of the silica is 4.0-8.0, preferably 5.5-8.0, and neutral, neutral weak acid or neutral weak alkaline silica is used as a carrier, so that the stability and activity of the loaded azelaic acid can be improved, the acidity of the azelaic acid can be improved, the pH value of the surface of the prepared composite powder is closer to the pH environment of the skin, the irritation to the skin is less, the health of the skin is more facilitated, and the composite powder is particularly suitable for sensitive skin.
In one embodiment, the azelaic acid solution is mixed with the silica by a stirring process at a speed of 1000r/min to 25000r/min. Specifically, azelaic acid solution and silica can be placed in a high-speed stirrer for stirring, so that the azelaic acid and the silica are fully mixed, and the loading effect of azelaic acid is improved.
In the step S3, the azelaic acid in the azelaic acid solution is subjected to drying treatment at a specific temperature, so that the azelaic acid in the azelaic acid solution has a certain crystallization rate, and the crystallization size is regulated and controlled, so that the azelaic acid is uniformly precipitated and loaded on the surface of silica in a recrystallization mode, the particle problem of the azelaic acid is effectively improved, the utilization rate and skin feel effect of the azelaic acid are improved, the application field of the azelaic acid is greatly widened, the effective contact effect of the azelaic acid and skin is improved, and the skin care effect of the azelaic acid can be better exerted. In addition, the surface acid-base number of the prepared azelaic acid-silica composite powder is closer to the acid-base environment of the skin, does not contain solvents or other substance additives, has less irritation to the skin and is more beneficial to the health of the skin.
The uniformity mentioned above means that 90% or more of silica achieves azelaic acid loading in terms of the total azelaic acid-silica composite powder amount.
Because the solvent is preferably hot water, alcohol solvent or water-alcohol mixed solution with the temperature of 50-90 ℃, in one embodiment, the drying temperature is preferably 80-150 ℃ and the drying time is 1-6 hours, thereby realizing the volatilization and removal of the solution and the recrystallization of the azelaic acid, simultaneously obtaining pure azelaic acid-silica composite powder, effectively avoiding the influence of the solvent on the skin and being more beneficial to the health of the skin.
The present invention also provides an azelaic acid-silica composite powder prepared by the method for preparing azelaic acid-silica composite powder as described above, which comprises silica and azelaic acid attached to the surface of the silica. In the azelaic acid-silica composite powder, more than 90% of silica realizes azelaic acid loading, so that the azelaic acid-silica composite powder has excellent loading uniformity.
On one hand, the azelaic acid-silica composite powder provided by the invention effectively avoids the problems of obvious granular feel and poor skin feel generated when solid azelaic acid is directly added; on the other hand, the problem that the solvent selection is limited because the azelaic acid is insoluble in common grease in the formula when the azelaic acid is added after being dissolved is effectively avoided, and the problems of granular feel and skin feel influence of the azelaic acid are effectively solved by loading the azelaic acid on the silica surface commonly added in the cosmetic formula, so that the application field of the azelaic acid is greatly widened.
At the same time, the grain diameter of the azelaic acid particles is obviously reduced, the azelaic acid particles are uniformly and firmly loaded on the surface of silica, the contact with the skin is more sufficient, the effect of the azelaic acid particles is more easily and fully exerted, and therefore, the addition amount of the azelaic acid required for achieving the effect is less.
In one embodiment, the particle size ratio of azelaic acid to silica is from 1:10 to 1:3.
The volume of the azelaic acid particles is smaller than that of the silica particles, and the good coating of the azelaic acid is realized on the premise of not affecting the properties of the silica such as skin feel, fluidity and the like, and meanwhile, the problem of poor skin feel of the azelaic acid is reduced.
The invention also provides application of the azelaic acid-silica composite powder in a make-up product.
Specifically, azelaic acid-silica composite powder can be added into loose powder and powder cake, and on the basis of the original skin feel regulator and adsorbent, the cosmetic powder also has the effects of acne removal, whitening, inflammation diminishing, bacteriostasis, oil control and skin care, and is more beneficial to realizing the combination of make-up and nourishing of make-up products.
It should be noted that the azelaic acid-silica composite powder of the present invention may be used mainly in solid cosmetics and also in emulsion, essence and other skin care products.
The azelaic acid-silica composite powder and the preparation method and application thereof will be further described by the following specific examples.
Example 1
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:8, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 27g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:100) into the high-speed stirrer, stirring at 5000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 2
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:4, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 25g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 1:20) into the high-speed stirrer, stirring at 5000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 2 an image of a scanning electron microscope of azelaic acid-silica composite powder prepared using azelaic acid shown in fig. 1 and silica shown in fig. 2 is shown in fig. 4, wherein the scale length of fig. 4 (a) is 5 μm and the scale length of fig. 4 (b) is 100 μm. By comparing fig. 3 and 4, it can be seen that azelaic acid in the azelaic acid-silica composite powder has been successfully supported on the silica surface; as can be seen from FIG. 4 (a), azelaic acid is completely loaded on the surface of silica, and is uniformly distributed, the size of azelaic acid particles is obviously smaller than that of silica, and the azelaic acid particles are in an irregular shape, so that the effect on the skin feel of the silica is small, and the silica has the skin care effects of whitening, acne removal and the like; as can be seen from FIG. 4 (b), azelaic acid realizes loading of 99% or more of silica particles, and azelaic acid has uniformity of loading of silica.
Example 3
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:5, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 36g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:50) into the high-speed stirrer, stirring at 10000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 4
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:4, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 35g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 7:100) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 5
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:3, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 32g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 2:25) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 6
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:2, and then 100g of azelaic acid solution with the specific surface area of 109.3m 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 27g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 9:100) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 7
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:2, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 30g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 1:10) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 8
Azelaic acid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:1, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 30g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:20) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 9
Azelaic acid and 75% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:1, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 40g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 1:5) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 120 ℃ oven for 3 hours, and cooling to obtain azelaic acid-silica composite powder.
Example 10
Will be nongDiacid and 95% alcohol are prepared into azelaic acid solution according to the mass ratio of 1:8, and then 100g of azelaic acid solution with the specific surface area of 112.6m is prepared 2 Placing/g silica with surface pH of 6.69 in a high-speed stirrer, uniformly spraying 27g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:100) into the high-speed stirrer, stirring at 10000r/min for 30s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Comparative example 1
5g of azelaic acid and 100g of silica (i.e. the mass ratio of azelaic acid to silica is 1:20) are placed in a high-speed stirrer, the specific surface area of the silica is 109.3m 2 And (3) stirring the mixture fully to obtain a mixture with the surface pH of 6.70, wherein the stirring speed is 20000r/min, the stirring time is 15s, heating and drying the mixture in a drying oven at 105 ℃ for 2 hours, and cooling the mixture to obtain the azelaic acid-silica composite powder.
Comparative example 1 solid azelaic acid was directly mixed with silica using azelaic acid shown in fig. 1 and silica shown in fig. 2, and it was seen from an image of azelaic acid under a 100-fold oil microscope in fig. 1 and an image of silica under a 100-fold oil microscope in fig. 2 that azelaic acid was excessively large in volume compared to silica, and it was difficult to achieve coating of silica with azelaic acid. By scanning electron microscopy images of the powder obtained, azelaic acid was found to be unsupported on the silica surface.
Comparative example 2
Azelaic acid and alcohol are prepared into azelaic acid solution according to the mass ratio of 1:4, and then 100g of azelaic acid solution with the specific surface area of 15.25m is prepared 2 Placing titanium dioxide with the surface pH value of 7.35 in a high-speed stirrer, uniformly spraying 25g of azelaic acid solution (namely, the mass ratio of azelaic acid to silica is 1:20) into the high-speed stirrer, stirring at the speed of 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain the azelaic acid-silica composite powder.
The scanning electron microscope image of the prepared powder material shows that the titanium dioxide powder has a slightly astringent skin feel, small specific surface area and large density, and has a limited effective load surface, and after being mixed with the azelaic acid solution, the powder material is easy to wet and agglomerate and difficult to uniformly mix, so that the azelaic acid has a poor load effect.
Comparative example 3
Azelaic acid and alcohol are prepared into azelaic acid solution according to the mass ratio of 1:9, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 30g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:100) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Comparative example 4
Azelaic acid and alcohol are prepared into azelaic acid solution according to the mass ratio of 2:1, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 4.5g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:100) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, heating and drying the mixture in a 105 ℃ oven for 2 hours, and cooling to obtain azelaic acid-silica composite powder.
Comparative example 5
Azelaic acid and alcohol are prepared into azelaic acid solution according to the mass ratio of 1:8, and then 100g of azelaic acid solution with the specific surface area of 109.3m is prepared 2 Placing/g silica with surface pH of 6.70 in a high-speed stirrer, uniformly spraying 27g azelaic acid solution (i.e. azelaic acid to silica mass ratio of 3:100) into the high-speed stirrer, stirring at 20000r/min for 15s, fully stirring to obtain a mixture, and naturally airing the mixture at room temperature to obtain azelaic acid-silica composite powder.
Azelaic acid raw material was used as blank 1, and the specific surface area was 109.3m 2 Silica with a surface pH of 6.70 was used as a blank 2 and the powder prepared in all examples, comparative examples and blanks were subjected to performance tests, the test indicators including pH, skin feel and azelaic acid loading of the powder.
The skin feel test method is to carry out blind skin feel test on the powder materials prepared in all examples, comparative examples and blank samples by 5 volunteers respectively, the test parts are faces and hands of the volunteers, the same amount of powder materials are taken, kneading is carried out for 10 seconds at a time, and evaluation (smooth, slick, rough, coarser and coarser) of granular feel of the powder materials used by 5 volunteers is counted.
The azelaic acid load rate test method is to take the weight of m 1 Uniformly mixing azelaic acid-silica composite powder with azelaic acid and silica in a mass ratio of x with alcohol according to a mass ratio of 1:4, filtering, washing, and drying filter cakes to obtain azelaic acid-silica composite powder with effective load, wherein the mass is m 2 Azelaic acid loading of 1- (m) 1 -m 2 )/[m 1× x/(1+x)]。
The results of the performance tests of the powders prepared in all examples, comparative examples and blanks are shown in Table 1.
TABLE 1
As can be seen from the test results in Table 1, under the same test conditions, the load rate of azelaic acid is significantly improved in examples 1 to 10 compared with comparative examples 1 to 5, which indicates that the load of azelaic acid on the silica surface can be effectively achieved by the preparation method of the present invention, and the load effect is good, and the skin feel of the prepared azelaic acid-silica composite powder is significantly better. Meanwhile, compared with blank 1, examples 1-10 realize that the pH value is closer to the acid-base environment of the skin, so that the skin irritation is smaller, the skin health is better, and the skin-care gel is particularly suitable for sensitive skin.
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 (10)
1. A method for preparing azelaic acid-silica composite powder, which is characterized by comprising the following steps:
mixing azelaic acid with a solvent to obtain an azelaic acid solution, wherein the mass ratio of the azelaic acid to the solvent is 1:1-1:8;
mixing the azelaic acid solution with silica to obtain a mixture;
and drying the mixture to obtain azelaic acid-silica composite powder, wherein the drying temperature is 10-80 ℃ higher than the volatilization temperature of the solvent.
2. The process for preparing azelaic acid-silica composite powder according to claim 1, wherein the mass ratio of azelaic acid to silica is 3:100 to 3:20.
3. The process for preparing azelaic acid-silica composite powder according to claim 1, wherein the specific surface area of the silica is not less than 100m 2 /g。
4. The process for preparing azelaic acid-silica composite powder according to claim 1, wherein the pH of the silica is 4.0 to 8.0.
5. The process for preparing azelaic acid-silica composite powder according to claim 1, wherein the mixing mode of azelaic acid solution and silica is selected from stirring treatment, and the rotation speed of stirring treatment is 1000 r/min-25000 r/min.
6. The method for producing azelaic acid-silica composite powder according to claim 1, wherein the solvent is at least one selected from hot water, an alcohol solvent or a hydroalcoholic mixture at a temperature of 50 ℃ to 90 ℃.
7. The process for preparing azelaic acid-silica composite powder according to claim 6, wherein the drying temperature is 80 to 150 ℃ and the drying time is 1 to 6 hours.
8. Azelaic acid-silica composite powder prepared by the process for preparing azelaic acid-silica composite powder according to any one of claims 1 to 7, wherein the azelaic acid-silica composite powder comprises silica and azelaic acid attached to the surface of the silica.
9. Azelaic acid-silica composite powder according to claim 8, characterized in that the particle size ratio of azelaic acid to silica is 1:10 to 1:3.
10. Use of the azelaic acid-silica composite powder according to claim 8 or claim 9 in a make-up product.
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