CN103385819B - Wax particles used in cosmetics and preparation method and application thereof in cosmetics - Google Patents
Wax particles used in cosmetics and preparation method and application thereof in cosmetics Download PDFInfo
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- CN103385819B CN103385819B CN201310273502.7A CN201310273502A CN103385819B CN 103385819 B CN103385819 B CN 103385819B CN 201310273502 A CN201310273502 A CN 201310273502A CN 103385819 B CN103385819 B CN 103385819B
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Abstract
The invention relates to wax particles used in cosmetics and a preparation method and an application thereof in cosmetics. The invention particularly relates to the wax particles used in cosmetics. The wax particles have a near-spherical shape, particle size of 10 to 1,000 mu m and contain 5% to 30% of dimethicone. The invention particularly relates to the preparation method of the wax particles and an application thereof in cosmetics.
Description
Technical field
The present invention relates to a kind of wax microgranule, its preparation method and the purposes of this wax microgranule in cosmetics.
Background technology
At present, commonly use powder stock or batching in external skin product, dental care product, spice, and so-called powder stock or batching comprise common inorganic powder in the art, as Talcum, Muscovitum, ferrous oxide etc.Along with the needs of development, also engender the unifonn spherical organic fine particles developed for overcoming inorganic powder deficiency, as synthetic polymer, natural polymer, encapsulated powder, composite powder etc.
The shape of particle of inorganic powder is granular, needle-like or irregularly shaped mostly, and completely spherical inorganic powder is extremely expensive in manufacturing cost, cosmetics, personal-care supplies, dental care product is applied very unrealistic.Granular, needle-like or erose inorganic powder grains sense of touch on skin proportion that is not good, that add himself comparatively large and cause dispersibility in the product bad and limit it and apply further.
Therefore, those skilled in the art and then have developed the organic dust that may be used for cosmetics, personal-care supplies, dental care product, such as natural polymer comprises cellulose, acetate fiber rope, silk-fibroin(s), chitin, de-second phthalein chitin etc.This natural polymer can be formed the character that globular powder and above-mentioned natural polymer powders have easily water suction by processing.
For the organic dust of cosmetics, personal-care supplies, dental care product, such as synthetic polymer microgranule comprises poly-phthalein amine, acrylate copolymer, polyethylene, crosslinked polystyrene, organosilicon polymer, fluorine based polymer, epoxy polymer, vinylidene chloride based polymer etc.Described synthetic polymer directly can be made spherical particle by adopting emulsion polymerization or suspension polymerisation or adopt distinct methods by synthetic polymer secondary operations globulate.Such as, patent application CN102348742A discloses a kind of organic silicone microparticle, this microgranule is rendered as on the whole and forms on the surface being equivalent to tetrahedral each the shape that peristome is the recess of circular, and this microgranule is by making the silanol group formative silicon compound of different chemical formula be hydrolyzed, and then under the aqueous conditions of base catalyst and anionic surfactant, occur that condensation reaction obtains.But obviously the manufacturing condition of these synthetic polymer microgranules is complicated, causes cost intensive and is difficult to use in production.
For the organic dust of cosmetics, personal-care supplies, dental care product, such as encapsulated powder comprises and is encapsulated in acrylic acid series polymeric compounds film by UV absorbent, spice, water, wet goods, keeps spherical state use or break in use and discharge UV absorbent, spice, water, wet goods encapsulated inside thing in formula for a product.
In addition, for the organic dust of cosmetics, personal-care supplies, dental care product, such as composite powder or composite particles comprise inorganic powder as titanium dioxide and synthetic polymer microgranule or natural polymer microgranule carry out combining and form composite powder.
But no matter above-mentioned inorganic powder or organic dust, still there is the various problems such as such as with high costs and/or complex process, therefore still need to further develop novel particle or powder to overcome the deficiencies in the prior art.
And then the applicant of the application notices, patent application CN1152336 discloses the mild cleaning soap containing smaller-sized particular wax, and in wherein said Wax particles, 85% to 100% size is less than 16 microns.In the disclosure in this patent, described Wax particles is by using foaming characteristic surfactant to disperse commercial wax, thus obtains Wax particles.But, because smaller-sized particular wax obtains in the presence of surfactants, cannot be separated from start to finish to obtain Wax particles.Correspondingly, this smaller-sized particular wax also can only be applied in this type surfactant product, and lacks the application prospect of independently wax microgranule.
To relate to or about the patent of the application of wax and silicone oil or patent application although the applicant of the application also notices in this area to have existed; particularly likely relate to fine wax particles or wax microgranule, but cause the comparatively complicated or cost intensive of condition technique due to the restriction of its reaction condition and be difficult to industrial application.
Such as, U.S. Patent application 6,843,982 are referred to and are applied in cosmetics and skin products by the mixture of silicone oil and wax, specifically, have employed the silicone oil of 5 ~ 97%, 3 ~ 50% Tissuemat E (PE wax) form non-water-soluble lipophilic phase, thus to be applied in lip pomade, end adornment, oily glue.In this application, be only that wax and silicone oil are individually joined in product as excipient, and the lipophilic phase preparation method described in this patent application cannot form wax microgranule or tiny Wax particles.
Again such as, the anhydrous topical formulation of polyphenol is disclosed in patent application CN1856293A, wherein this composition of matter comprises anhydrous topical frost, gel or cream base matter, polyphenol and suitable adsorbent binding carrier, describedly include simethicone in conjunction with in carrier, and described anhydrous topical is white, include wax in gel or cream.Even if but include simethicone and wax in the preparation of this patent application, but under the preparation condition recorded in this patent application, cannot Wax particles be obtained.
For another example a kind of Chinese medicine ointment and preparation method thereof for the treatment of burn, scalding is disclosed in patent application CN10112488A, this Chinese medicine ointment comprises following raw materials according and is prepared from: Radix Et Rhizoma Rhei, Cera Flava, Oleum Sesami and pharmaceutically acceptable substrate, described pharmaceutically acceptable substrate includes simethicone.Similarly, be not both disclosed in the disclosure in this patent and obtained wax microgranule by simethicone, and under the preparation condition recorded in this patent application, cannot obtain wax microgranule or tiny Wax particles yet.
The applicant of the application to find commercial wax not relate in the prior art by simethicone or makes waxed one-tenth wax microgranule by oneself, and the application of thus obtained wax microgranule in cosmetics.It is shocking that the application can be convenient and simple by waxed one-tenth wax microgranule only by simethicone, thus Simplified flowsheet complexity, and greatly reduce costs, meet the requirement in cosmetic applications simultaneously.
The information being disclosed in this background of invention technology part is only intended to deepen the understanding to general background technology of the present invention, and should not be regarded as admitting or imply in any form that this information structure has been prior art known in those skilled in the art.
Summary of the invention
A theme of the present invention is a kind of wax microgranule for cosmetics.Described wax microgranule is organic fine particles, and in almost spherical or spheroidal particle, this wax microgranule has 10 to 1000 microns, preferably 20 to 100 microns, more preferably the particle diameter of 10 to 70 microns, and described wax microgranule comprises the simethicone of 5 ~ 30%.In one embodiment, this wax microgranule is made up of the simethicone of wax and 5 ~ 30%.
Another theme of the present invention is the method preparing described wax microgranule, the method comprises: under simethicone existent condition, by wax through heating and melting, dispersion, cooled and solidified to form microgranule, after removing unnecessary simethicone subsequently, thus directly obtain wax microgranule.
In one embodiment, the concrete steps that the present invention prepares the method for Wax particles as above comprise: the temperature 1) simethicone of the wax of 1% ~ 90% mass fraction and 10 ~ 99% mass fractions being mixed and heated to 70 DEG C ~ 150 DEG C; 2) under the rotating speed of 20 ~ 350 revs/min, this mixture is stirred to being uniformly dispersed; 3) the lower continuous stirring of insulation 5 ~ 60 minutes; 4) under the condition stirred, cooling makes mixture solidify; 5) by simethicone unnecessary for gained mixture filtering and removing, thus wax microgranule is obtained.A little simethicone can be contained in wax microgranule of the present invention.
Summary, the preparation method of wax microgranule of the present invention under the existence of disperse medium, is frozen into tiny granule after being melted by wax.
Wax used in the present invention comprises Cera Flava, Cera Chinensis, spermaceti, haze tallow, palm wax, refined paraffin wax, microwax, rice bran wax, sugarcane wax, glyceryl monostearate etc.Described wax all can by commercially available or self-control and obtain.
Cera Flava used in the present invention is refining particles.In yellow, fallow or yellow-white, opaque or sub-translucent, smooth surface.Body is comparatively light, and waxiness, section sand shape, pinches can soften with hand rubbing.The fusing point of described Cera Flava is 62 ~ 65 DEG C.
Cera Chinensis used in the present invention is refining particles.In white or off-white color, surface smoothing, or slightly wrinkle, tool gloss.Body is light, and matter is firmly and slightly crisp, and afterturn is then pulverized.Section is strip or graininess.The fusing point of described Cera Chinensis is 81 ~ 85 DEG C.
Spermaceti used in the present invention is refining particles.In white, odorless is glossy.The fusing point of described spermaceti is 41 ~ 49 DEG C.
Haze tallow used in the present invention is refining particles.In white to micro-yellow particle, slightly special odor.The fusing point of described haze tallow is 50 ~ 53 DEG C.
Palm wax used in the present invention is refining particles.In light brown to lark, there is gentle special smell, almost tasteless.The fusing point of described palm wax is 81 ~ 88 DEG C.
Refined paraffin wax used in the present invention is refining particles.In white or faint yellow.The fusing point of described refined paraffin wax is 54 ~ 64 DEG C.
Microwax used in the present invention is refining particles.Be creamy white.The fusing point of described microwax is 68 ~ 72 DEG C.
Rice bran wax used in the present invention is refining particles.In faint yellow.The fusing point of described rice bran wax is 78 ~ 82 DEG C.
Sugarcane wax used in the present invention is refining particles.In brown-green to dark brown, matter is hard and crisp.The fusing point of described sugarcane wax is 74 ~ 82 DEG C.
Glyceryl monostearate used in the present invention is White waxy thin slice or beadlet solid.The fusing point of described glyceryl monostearate is 55 ~ 60 DEG C.
The present invention uses simethicone as dispersant, and it is commercial goods.Simethicone, to human non-toxic's property, is not also decomposed by body fluid, is conventional cosmetic material, wide material sources and convenient.The present invention selects simethicone as the dispersant of wax, and its range of viscosities is 10 ~ 500000 centipoises, and preferred range of viscosities is 50 ~ 10000 centipoises, and most preferred range of viscosities is 100 ~ 5000 centipoises.
In the preparation process in accordance with the present invention, the content of wax and simethicone is the wax of 1% ~ 90% mass fraction and the simethicone of 10 ~ 99% mass fractions, preferred content is the wax of 2% ~ 70% mass fraction and the simethicone of 30 ~ 98% mass fractions, and most preferred content is the wax of 5 ~ 60% mass fractions and the simethicone of 40 ~ 95% mass fractions.
In the preparation process in accordance with the present invention, wax and simethicone are heated to 70 DEG C ~ 150 DEG C, preferably 80 ~ 130 DEG C, the most preferably temperature range of 90 ~ 120 DEG C.
In the preparation process in accordance with the present invention, make the mixture of wax and simethicone be 20 ~ 350 revs/min, preferably 40 ~ 300 revs/min, most preferably carry out disperseing until be uniformly dispersed under 50 ~ 200 revs/min of ranges of speeds.
In the preparation process in accordance with the present invention, by the mixture of wax and simethicone at 70 DEG C ~ 150 DEG C, preferably 80 ~ 130 DEG C, most preferably continuous stirring 5 ~ 60 minutes in the temperature range of 90 ~ 120 DEG C, preferably 10 ~ 40 minutes, most preferably 15 ~ 30 minutes.
In the preparation process in accordance with the present invention, after by the mixture insulated and stirred of wax and simethicone, less than 40 DEG C are cooled to, preferred cool to room temperature.
In the preparation process in accordance with the present invention, the mode by filtering removes unnecessary simethicone.Filter method both can natural filtration, vacuum filtration, also can centrifugal filtration, preferred method is vacuum filtration or centrifugal filtration.
The wax microgranule obtained by method of the present invention, its particle diameter range is 10 ~ 1000 microns.
The wax microgranule obtained by method of the present invention, wherein the content of simethicone is about 5 ~ 30%.
Wax microgranule of the present invention had both been different from the irregular contour that inorganic powder has, and also overcomed the shortcoming that traditional natural polymer microgranule is not easily preserved, thus made wax microgranule method for making involved in the present invention simple, practical.Meanwhile, with the organic fine particles of other type, such as synthetic polymer microgranule, encapsulated powder, composite powder or composite particles are compared, and the raw material of this wax microgranule can be obtained by commercial acquisition or self-control, wide material sources.The present application has raw material sources convenience, the simple feature of method for making.
Wax microgranule of the present invention can be used in cosmetics, external skin product, personal-care supplies, dental care product or spice etc.
Wax microgranule of the present invention can be applied in cleansing milk product.Carry out preparing burden according to the known preparation method of cleansing milk, sterilize, mix or homogenizing, through be cooled to be no more than 45 DEG C of conditions under add 5 ~ 25% wax microgranule, make the cleansing milk used for cosmetic with deep layer cleaning effect after fully stirring.In one embodiment, the additional proportion of preferred wax microgranule is 10 ~ 20%.
Wax microgranule of the present invention also can be applied in cleansing cream product.Prepare cleansing cream according to the method in the invention process example, be no more than the wax microgranule adding 5 ~ 25% under the condition of 45 DEG C, after fully stirring, making the cleansing cream used for cosmetic with deep layer cleaning effect.In one embodiment, the additional proportion of preferred wax microgranule is 10 ~ 20%.
Wax microgranule of the present invention also can be applied in massage oil product.Prepare massage oil according to the method in the invention process example, be no more than the wax microgranule adding 5 ~ 25% under the condition of 45 DEG C, after fully stirring, making massage oil.In one embodiment, the additional proportion of preferred wax microgranule is 10 ~ 20%.
Wax microgranule of the present invention can be applied in massage cream product.Prepare massage cream according to the method in the invention process example, be no more than the wax microgranule adding 5 ~ 25% under the condition of 45 DEG C, after fully stirring, making massage cream.In one embodiment, the additional proportion of preferred wax microgranule is 10 ~ 20%.
The fine particle of wax microgranule of the present invention under the microscope in almost spherical, have round and smooth, without the feature such as corner angle, matter is soft, not injured skin when being applied to skin surface grinding, play the effect of Exfoliating Scrub and skin dirt, be convenient to the dirt in Peppermint Extract, concavo-convex position, reach skin depth skin clean, or rub massage effect, the blood circulation of skin can be increased.In addition, in wax microgranule involved in the present invention, the wax used relates to multiple natural animal wax, as Cera Flava, Cera Chinensis etc., containing abundant nutrient substance, as: flavone, long-chain fatty alcohol etc., reach the effect of maintaining skin.
By include in accompanying drawing herein and subsequently together with accompanying drawing for illustration of the detailed description of the invention of some principle of the present invention, the further feature that method of the present invention has and advantage will become to be known or is more specifically illustrated.
Accompanying drawing explanation
Fig. 1 is the photo of the Cera Flava microgranule that obtains according to embodiment 1 (400 times) under the microscope.
Fig. 2 is the photo of the Cera Chinensis microgranule that obtains according to embodiment 2 (400 times) under the microscope.
Fig. 3 is the photo of the spermaceti microgranule that obtains according to embodiment 3 (400 times) under the microscope.
Fig. 4 is the photo of the Chinese haze tallow microgranule that obtains according to embodiment 4 (400 times) under the microscope.
Fig. 5 is the photo of the palm wax microgranule that obtains according to embodiment 5 (400 times) under the microscope.
Fig. 6 is the photo of the refined paraffin wax microgranule that obtains according to embodiment 6 (400 times) under the microscope.
Fig. 7 is the photo of the microwax microgranule that obtains according to embodiment 7 (400 times) under the microscope.
Fig. 8 is the photo of the rice bran wax microgranule that obtains according to embodiment 8 (400 times) under the microscope.
Fig. 9 is the photo of the glyceryl monostearate microgranule that obtains according to embodiment 9 (400 times) under the microscope.
Figure 10 is the photo of the Cera Flava microgranule that obtains according to embodiment 10 (400 times) under the microscope.
Figure 11 is the photo of the Cera Flava microgranule that obtains according to embodiment 11 (400 times) under the microscope.
Figure 12 is the photo of the ointment that obtains according to comparative example 1 (400 times) under the microscope.
Figure 13 is the photo of the not clean skin of ala nasi of (200 times) under skin detection instrument as described in example 16 above.
Figure 14 is the photo of the skin of ala nasi after the cleansing milk of the non-content of wax microgranule of use of (200 times) under skin detection instrument as described in example 16 above cleans.
Figure 15 is the photo of the skin of ala nasi after the use of (200 times) under skin detection instrument is as described in example 16 above cleaned containing the cleansing milk of Cera Flava microgranule.
Figure 16 is the photo of the not clean skin of ala nasi of (200 times) under skin detection instrument as described in example 16 above.
Figure 17 is the photo of the skin of ala nasi after the cleansing cream of the non-content of wax microgranule of use of (200 times) under skin detection instrument as described in example 16 above cleans.
Figure 18 is the photo of the skin of ala nasi after the use of (200 times) under skin detection instrument is as described in example 16 above cleaned containing the cleansing cream of Cera Flava microgranule.
Figure 19 is the photo of the inner forearm skin of (200 times) under skin detection instrument as described in example 16 above.
Figure 20 is that the photo of the inner forearm skin after 5 minutes massaged by the massage oil of the non-content of wax microgranule of use of (200 times) under skin detection instrument as described in example 16 above.
Figure 21 is that the photo of the inner forearm skin after 5 minutes is massaged in the use of (200 times) under skin detection instrument as described in example 16 above containing the massage oil of Cera Flava microgranule.
Figure 22 is the photo of the inner forearm skin of (200 times) under skin detection instrument as described in example 16 above.
Figure 23 is that the massage cream of the non-content of wax microgranule of use of (200 times) under skin detection instrument as described in example 16 above massages the photo of the inner forearm skin after 5 minutes.
Figure 24 is that the photo of the inner forearm skin after 5 minutes is massaged in the use of (200 times) under skin detection instrument as described in example 16 above containing the massage cream of Cera Flava microgranule.
Detailed description of the invention
The present invention uses the simethicone of different viscosities as the dispersant of wax microgranule, comprise viscosity and be respectively the simethicone that 10,50,100,350,500,1000,5000,10000,200000,500000 centipoises amount to 10 kinds, raw material using Cera Flava as wax microgranule, charge ratio is Cera Flava 30% mass fraction, simethicone 70% mass fraction, and preparation in accordance with the present invention prepares wax microgranule.Being heated under 90 ~ 120 DEG C of conditions, according to the difference of simethicone viscosity, regulating mixing speed 50 ~ 350 revs/min to be uniformly dispersed in simethicone to make the Cera Flava melted, and avoiding layering.Then Keep agitation 5 to 60 minutes at such a temperature, is cooled to 40 ° of below C, preferred room temperature subsequently, after filtering, obtains Cera Flava microgranule under the condition stirred.The simethicone that viscosity is respectively 10,50,100,350,500,1000,5000,10000,200000,500000 centipoises all can obtain Cera Flava microgranule as dispersant.The Cera Flava microgranule obtained is examined under a microscope as graininess, and particle diameter is slightly different according to the difference of simethicone viscosity, and its particle diameter range is about 10 ~ 1000 microns.When the simethicone of viscosity 50 ~ 10000 centipoise is as dispersant, the particle diameter of Cera Flava microgranule is 10 ~ 120 microns.Viscosity be the simethicone of 350 ~ 5000 centipoises as dispersant time, the particle diameter of Cera Flava microgranule is 10 ~ 100 microns.Above-mentioned Cera Flava microgranule hands all has granular sensation in various degree when twisting with the fingers.
In the present invention, the commercial waxs such as Cera Flava, Cera Chinensis, spermaceti, haze tallow, palm wax, refined paraffin wax, microwax, rice bran wax, sugarcane wax, glyceryl monostearate or wax analog can be used to carry out the preparation of wax microgranule.
The viscosity of simethicone used in the following example is respectively 350 centipoises and 1000 centipoises.The simethicone of the wax of 20 ~ 30% mass fractions and 70 ~ 80% mass fractions is mixed, is heated to wax and melts.Heating-up temperature is generally set in more than wax fusing point 20 ~ 40 DEG C for best.Regulate mixing speed 60 ~ 200 revs/min, the wax melted is uniformly dispersed in simethicone, avoids layering.Under the condition stirred, be cooled to room temperature, after filtering, obtain wax microgranule.The commercial wax that the present invention selects and class commercial wax, comprise Cera Flava, Cera Chinensis, spermaceti, haze tallow, palm wax, refined paraffin wax, microwax, rice bran wax, sugarcane wax, glyceryl monostearate etc., all prepared wax microgranule of the present invention.
In the following embodiment of the present invention, the wax of assistant ingredients proportionate relationship and simethicone is selected to carry out the preparation of wax microgranule.The present invention selects viscosity to be the simethicone of 1000 centipoises, originate as wax using Cera Flava, selected mass fraction than the Cera Flava being respectively 5:95,10:90,20:80,30:70,40:60,50:50,60:40,70:30,80:20,90:10 respectively: simethicone carries out the preparation of Cera Flava microgranule.Be heated to 110 DEG C, regulate mixing speed 60 ~ 200 revs/min, the Cera Flava melted is uniformly dispersed in simethicone, avoids layering.Under well-beaten condition, be cooled to room temperature, after filtering, obtain wax microgranule of the present invention.
Embodiment
Embodiment 1: the preparation of Cera Flava microgranule
The Cera Flava of 15.0 kilograms, the simethicone (viscosity 1000 centipoise) of 35.0 kilograms join in retort, be heated to 110 DEG C, use the anchor agitator of band scraping to stir 20 minutes with the speed of 90 revs/min, be creamy white by the material in the observing response tank of visualization hole.Keep mixing speed and be cooled to less than 45 DEG C, discharging, being transferred in the double-deck high density terylene filter-cloth filtering bag in drum-type tripod pendulum type batch centrifugal, centrifugal 30 minutes with 1400 revs/min, to remove unnecessary simethicone, obtain 18.6 kilograms of Cera Flava microgranules.Gained Cera Flava microgranule is stored in cleaning container for subsequent use.
A little wax particulate homogenous is coated in clean glass slide, covered, namely makes wax microgranule smear.Eyepiece micrometer is placed in microscope ocular, stage micrometer is placed on dressing table, observe under actual observation amplification condition and calculate the physical length corresponding to eyepiece micrometer scale.Observe under wax microgranule smear is placed in dressing table, record the eyepiece micrometer number of division corresponding to 40 ~ 50 wax microgranules, calculate the actual particle diameter range of its correspondence.The particle diameter range of the Cera Flava microgranule of gained is 20 ~ 60 microns, and microscope hypograph is shown in Fig. 1.
Embodiment 2: the preparation of Cera Chinensis microgranule
The Cera Chinensis of 150 grams, the simethicone (viscosity 1000 centipoise) of 350 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 120 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 20 minutes with the speed of 100 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain the Cera Chinensis microgranule of 180 grams.Gained wax microgranule is stored in cleaning container for subsequent use.
By Cera Chinensis microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained Cera Chinensis microgranule is 20 ~ 100 microns, and microscope hypograph is shown in Fig. 2.
Embodiment 3: the preparation of spermaceti microgranule
The spermaceti of 150 grams, the simethicone (viscosity 350 centipoise) of 350 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 90 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 20 minutes with the speed of 80 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 179 grams of spermaceti microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By spermaceti microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained spermaceti microgranule is 20 ~ 100 microns, and microscope hypograph is shown in Fig. 3.
Embodiment 4: the preparation of haze tallow microgranule
The Chinese haze tallow of 100 grams, the simethicone (viscosity 1000 centipoise) of 400 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 100 DEG C, use blade agitator to stir with the speed of 100 revs/min 20 minutes to mixture to be the emulsion form of yellowish.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus class yellow mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 113 grams of haze tallow microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By haze tallow microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained haze tallow microgranule is 80 ~ 1000 microns, and microscope hypograph is shown in Fig. 4.
Embodiment 5: the preparation of palm wax microgranule
The palm wax of 100 grams, the simethicone (viscosity 1000 centipoise) of 400 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, use blade agitator to stir with the speed of 100 revs/min 20 minutes to mixture to be the emulsion form of class yellow.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus class yellow mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 109 grams of palm wax microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By palm wax microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained palm wax microgranule is 10 ~ 70 microns, and microscope hypograph is shown in Fig. 5.
Embodiment 6: the preparation of refined paraffin wax microgranule
The refined paraffin wax of 150 grams, the simethicone (viscosity 1000 centipoise) of 350 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 20 minutes with the speed of 120 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 184 grams of refined paraffin wax microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By refined paraffin wax microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained refined paraffin wax microgranule is 10 ~ 40 microns, and microscope hypograph is shown in Fig. 6.
Embodiment 7: the preparation of microwax microgranule
The microwax of 100 grams, the simethicone (viscosity 350 centipoise) of 400 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, and using blade agitator to stir 20 minutes with the speed of 100 revs/min is linen emulsion form to mixture.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus pale white mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 119 grams of microwax microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By microwax microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained microwax microgranule is 10 ~ 80 microns.Microscope hypograph is shown in accompanying drawing 7.
Embodiment 8: the preparation of rice bran wax microgranule
The rice bran wax of 100 grams, the simethicone (viscosity 350 centipoise) of 400 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, and using blade agitator to stir 20 minutes with the speed of 100 revs/min is flaxen emulsion form to mixture.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus pale yellow mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 120 grams of rice bran wax microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By rice bran wax microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained rice bran wax microgranule is 10 ~ 80 microns, and microscope hypograph is shown in Fig. 8.
Embodiment 9: the preparation of glyceryl monostearate microgranule
The glyceryl monostearate of 150 grams, the simethicone (viscosity 350 centipoise) of 350 grams join in 1000 milliliter of three neck round-bottomed flask, be heated to 110 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 20 minutes with the speed of 100 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 183 grams of glyceryl monostearate microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By glyceryl monostearate microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained glyceryl monostearate microgranule is 10 ~ 70 microns, and microscope hypograph is shown in Fig. 9.
Embodiment 10: the preparation of Cera Flava microgranule
The Cera Flava of 25 grams, the simethicone (viscosity 1000 centipoise) of 475 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 20 minutes with the speed of 100 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 31 grams of Cera Flava microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By Cera Flava microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained Cera Flava microgranule is 10 ~ 40 microns, and microscope hypograph is shown in Figure 10.
Embodiment 11: the preparation of Cera Flava microgranule
The Cera Flava of 450 grams, the simethicone (viscosity 1000 centipoise) of 50 grams join in 1000 milliliter of three neck round-bottomed flask, are heated to 110 DEG C, use blade agitator to stir the emulsion form be creamy white to mixture for 30 minutes with the speed of 200 revs/min.Keep mixing speed and be cooled to less than 45 DEG C, obtaining outer appearnce like unguinosus opalescent mixture.With buchner funnel double-layer filter paper sucking filtration to remove unnecessary simethicone, obtain 482 grams of Cera Flava microgranules.Gained wax microgranule is stored in cleaning container for subsequent use.
By Cera Flava microgranule as described in Example 1 step make smear, examine under a microscope.The particle diameter range of thus obtained Cera Flava microgranule is 10 ~ 50 microns, and microscope hypograph is shown in Figure 11.
Embodiment 12: containing the cleansing milk of Cera Flava microgranule
1.5 kilograms of Oleum Sesami, 1.5 kg of carbon ten six-ten eight fatty alcohol, 0.5 kilogram of iso-octyl palmitate, 0.4 kilogram of ceteareth-2,0.25 kilogram of vitamin E, 0.12 kilogram of hexadecanyl phosphate potassium salt are put into oil phase tank, airtight, stir with the rotating speed of 60 revs/min, keep this mixing speed to discharging.The mixture of gained is heated to 85 DEG C, is incubated 60 minutes.
0.12 kilogram of xanthan gum is dispersed in 4 kilograms of glycerol, joins in aqueous phase tank.Add 25 kilograms of Radix et Caulis Opuntiae Dillenii juices, 6 kilograms of C12-16 alkyl polyglucoside, 3 kilograms of N-lauroyl propylhomoserin sodium salts, 3 kilograms of cocamido propyl betaine, 0.6 kilogram of ceteareth-21,0.5 kilogram of lactalbumin, 0.05 kilogram of EDETATE SODIUM respectively.Airtight, stir with the rotating speed of 60 revs/min, keep this mixing speed to discharging.Be heated to 75 DEG C, be incubated 60 minutes.
Emulsion tank is preheated to 75 DEG C, evacuation makes vacuum reach 0.07MPa.Filtered through 100 orders by 2/3 aqueous phase material in aqueous phase tank, be transferred in emulsion tank, open the agitator in emulsion tank, stir with the rotating speed of 60 revs/min, this mixing speed is retained to formation mixture.Successively the whole material in oil phase tank and remaining aqueous phase material are gone in emulsion tank through 100 order filters; Be evacuated to vacuum and reach 0.04MPa; Homogenizing 2 times (homogenizing speed setting 3000rpm), each 7 minutes, 5 minutes, interval, was incubated 75 DEG C.
First the mixture in emulsion tank is cooled to 65 DEG C, is evacuated to 0.06MPa, insulation homogenizing 8 minutes.
And then the mixture in emulsion tank is cooled to 45 DEG C, be evacuated to 0.08MPa, add 0.5 kilogram of essence, homogenizing 7 minutes.
Finally add the Cera Flava microgranule 7 kilograms obtained in the embodiment of the present invention 1,60 revs/min are stirred 20 minutes.
Be cooled to room temperature, to obtain cleansing milk in discharging to clean container.Thus obtained cleansing milk is detected through sampling, carries out the item inspections such as stability, pH, microorganism; After indices is all qualified, require that fill is in aluminium-plastic pipe according to loading amount; After packaging process, cleansing milk finished product.
Embodiment 13: containing the cleansing cream of Cera Flava microgranule
By 800 grams of propylene glycol, 400 grams of glycerol, 800 gram of 35% potassium hydroxide solution, 80 gram of 20% sodium hydroxide solution, 320 grams of tetradecylic acids, 80 grams of hexadecylic acids, 80 grams of stearic acids, 160 grams of dodecoic acids, 60 grams of glyceryl monostearates, 80 grams of Radix et Caulis Opuntiae Dillenii juices, 40 grams of tween 20s, 1 gram 2,6-ditertbutylparacresol puts into retort, open and stir, rotating speed 60 revs/min, and be retained to discharging, be heated to 70 DEG C, be stirred to whole dissolving.
Retort raw material is gone in emulsion tank through 100 order filters, opens and stir, rotating speed 60 revs/min, and be retained to discharging; Be evacuated to 0.04MPa, be heated to 80 DEG C, insulated and stirred 50 minutes.
And then in emulsion tank, add 40 grams of salicylic acid, stir 3 minutes; Add 10 grams of octyl group glycine, stir 3 minutes; Add 20 grams of vitamin B6 acid dipalmitates, stir 4 minutes.With 2000rpm homogenizing 3 minutes.
Be cooled to 45 DEG C subsequently, add the Cera Flava microgranule obtained in 550 grams of embodiment of the present invention 1,20 grams of plants essential oils in emulsion tank, 60 revs/min are stirred 15 minutes.
Be cooled to room temperature, to obtain cleansing cream in discharging to clean container.Thus obtained cleansing cream is detected through sampling, carries out the item inspections such as stability, pH, microorganism; After indices is all qualified, require that fill is in aluminium-plastic pipe according to loading amount; After packaging process, cleansing cream finished product.
Embodiment 14: containing the massage oil of Cera Flava microgranule
1500 grams of Oleum Sesami, 1500 grams of olive oil, 100 grams of vitamin Es are added in vacuum tank, are evacuated to vacuum and reach 0.06MPa.Heated and stirred to 85 DEG C, mixing speed 50 revs/min, and insulated and stirred 50 minutes.
Then be cooled to 45 DEG C, add 200 grams of quintessence oils, 550 grams of Cera Flava microgranules (from the embodiment of the present invention 1), 70 grams of vitamin C fat acid esters, 0.3 gram of vitamin A in vacuum tank, 50 revs/min are stirred 20 minutes.
Be down to room temperature, to obtain massage oil in discharging to clean container.Thus obtained massage oil is detected through sampling, carries out the item inspections such as stability, pH, microorganism; After indices is all qualified, require that fill is in glass container according to loading amount; After packaging process, massage oil finished product.The massage oil of this Cera Flava microgranule belongs to the frosted massage oil product that market is commonly called as.
Embodiment 15: containing the massage cream of Cera Flava microgranule
2600 grams of Oleum Sesami, 350 grams of Cera Flavas, 100 grams of vitamin Es are added in vacuum tank, are evacuated to vacuum and reach 0.06MPa.Heated and stirred to 85 DEG C, mixing speed 50 revs/min, and insulated and stirred 50 minutes.
Then be cooled to 65 DEG C, in vacuum tank, add 180 grams of quintessence oils, 0.3 gram of vitamin A, stir 20 minutes.
Be cooled to 45 DEG C subsequently, add 500 grams of Cera Flava microgranules (from the embodiment of the present invention 1), 70 grams of vitamin C fat acid esters in vacuum tank, 50 revs/min are stirred 20 minutes.
Be cooled to room temperature, to obtain massage cream in discharging to clean container.Thus obtained massage cream is detected through sampling, carries out the item inspections such as stability, pH, microorganism; After indices is all qualified, require that fill is in glass container according to loading amount; After packaging process, massage cream finished product.
Comparative example 1:
Described ointment is obtained according to the method for embodiment two in patent application CN10112488A.By gained ointment as described in Example 1 step make smear, be placed in basis of microscopic observation, see Figure 12.As shown in figure 12, wherein dark filament is wax crystallization, and tiny pointing object is medicinal residues sample particulate matter, does not observe the formation of Wax particles.
Embodiment 16: dermal application contrast test between content of wax micronize cosmetic and corresponding not content of wax micronize cosmetic
1, test material
The cosmetic sample source of dermal application contrast test:
(1) containing the cleansing milk of Cera Flava microgranule from the embodiment of the present invention 12.
(2) the cleansing milk of content of wax microgranule is not prepared, uniquely unlike not adding Cera Flava microgranule according to the method for making described in the embodiment of the present invention 12.
(3) containing the cleansing cream of Cera Flava microgranule from the embodiment of the present invention 13.
(4) the cleansing cream of content of wax microgranule is not prepared, uniquely unlike not adding Cera Flava microgranule according to the method for making described in the embodiment of the present invention 13.
(5) containing the massage oil of Cera Flava microgranule from the embodiment of the present invention 14.
(6) the massage oil of content of wax microgranule is not prepared, uniquely unlike not adding Cera Flava microgranule according to the method for making described in the embodiment of the present invention 14.
(7) containing the massage cream of Cera Flava microgranule from the embodiment of the present invention 15.
(8) the massage cream of content of wax microgranule is not prepared, uniquely unlike not adding Cera Flava microgranule according to the method for making described in the embodiment of the present invention 15.
Dermal application contrast test adopts BV2106U type hair/skin detection instrument (being equipped with 200 times of enlarging lens) to observe, and for recording the skin appearance image of local after tuerculoderma, is used for the effect of differentiation different product with this.
2, tested object
5 volunteers are selected to carry out skin contrast test, one full year of life at age 26 to 60.
3, the operational approach of dermal application contrast test
(1) cleansing milk contrast test: the skin first detecting wing of nose both sides with hair/skin detection instrument, record image.The left side wing of nose smears the appropriate cleansing milk sample containing Cera Flava microgranule, the right side wing of nose is smeared the cleansing milk sample of the not content of wax microgranule of equivalent, smear 1 minute gently respectively, use hair/skin detection instrument record skin appearance image with after napkin wiped clean.
(2) massage oil contrast test: first detect inboard arm skin with hair/skin detection instrument, record image.Smear the appropriate massage oil sample containing Cera Flava microgranule inside left arm, smear the massage oil sample of the not content of wax microgranule of equivalent inside right arm, smear 5 minutes gently respectively, use hair/skin detection instrument record skin appearance image with after napkin wiped clean.
(3) cleansing cream contrast test: the skin first detecting wing of nose both sides with hair/skin detection instrument, record image.The left side wing of nose smears the appropriate cleansing cream sample containing Cera Flava microgranule, the right side wing of nose is smeared the cleansing cream sample of the not content of wax microgranule of equivalent, smear 1 minute gently respectively, use hair/skin detection instrument record skin appearance image with after napkin wiped clean.
(4) massage cream contrast test: first detect inboard arm skin with hair/skin detection instrument, record image.Smear the appropriate massage cream sample containing Cera Flava microgranule inside left arm, smear the massage cream sample of the not content of wax microgranule of equivalent inside right arm, smear 5 minutes gently respectively, use hair/skin detection instrument record skin appearance image with after napkin wiped clean.
4, comparative test result
4.1, cleansing milk uses contrast test
First detect the skin of wing of nose both sides with hair/skin detection instrument, see Figure 13.Compared with wing of nose area skin (see Figure 15) after wing of nose area skin (see Figure 14) after using the cleansing milk not containing Cera Flava microgranule to clean cleans with the cleansing milk of content of wax microgranule, the effect of use containing the dirt and blackhead of dispelling of removing pore and other jog position after the cleansing milk of Cera Flava microgranule is more obvious.
Can observe from Figure 13, the visible significantly blackhead at pore place.Can observe from Figure 14, still have recognizable pollutant.Can observe from Figure 15, after using the cleansing milk containing Cera Flava microgranule, local skin has no obvious pollutant.
4.2, cleansing cream uses contrast test
First detect the skin of wing of nose both sides with hair/skin detection instrument, see Figure 16.Compared with wing of nose area skin (see Figure 18) after wing of nose area skin (see Figure 17) after using the cleansing cream not containing Cera Flava microgranule to clean cleans with the cleansing cream of content of wax microgranule, the effect of use containing the dirt and blackhead of dispelling of removing pore and other jog position after the cleansing cream of Cera Flava microgranule is more obvious.Can observe from Figure 16, the visible significantly blackhead at pore place.Can observe from Figure 17, still have the attachment of recognizable " dead bark " sample.Can observe from Figure 18, after using the cleansing cream containing Cera Flava microgranule, local skin has no obvious pollutant.
4.3, massage oil uses contrast test
First detect inboard arm skin with hair/skin detection instrument, see Figure 19.Compared with inner forearm skin (see Figure 21) after using the inner forearm skin (see Figure 20) of the massage oil not containing Cera Flava microgranule to massage with the massage oil of content of wax microgranule, use the inner forearm skin after the massage of the massage oil containing Cera Flava microgranule to seem ruddy, and it is glossy more to seem.
Can observe from the contrast of Figure 19 ~ Figure 21, use as shown in figure 21 seems ruddy than the skin after the massage oil massage of same use non-content of wax microgranule as shown in figure 20 containing the inner forearm skin after the massage oil massage of Cera Flava on apparent, points out the blood circulation of its local skin to obtain enhancing; Equally, the inner forearm skin after containing the massage oil massage of Cera Flava is used more to seem glossy than the skin after using the massage oil of non-content of wax microgranule to massage equally on apparent.
4.4, massage cream use contrast test
First detect inboard arm skin with hair/skin detection instrument, see Figure 22.Compared with inner forearm skin (see Figure 24) after using the inner forearm skin (see Figure 23) after the massage of the massage cream not containing Cera Flava microgranule to massage with the massage cream of content of wax microgranule, use the inner forearm skin after the massage of the massage cream containing Cera Flava microgranule to seem ruddy, and it is glossy more to seem.
Can observe from the contrast of Figure 22 ~ Figure 24, use the inner forearm skin after containing the massage cream massage of Cera Flava to seem ruddy than the skin after the massage cream massage of same use non-content of wax microgranule as shown in figure 23 as of fig. 24 on apparent, point out the blood circulation of its local skin to obtain enhancing; Equally, the inner forearm skin after containing the massage cream massage of Cera Flava is used more to seem glossy than the skin after using the massage cream of non-content of wax microgranule to massage equally on apparent.
Claims (14)
1., for a wax microgranule for cosmetics, it is characterized in that described wax microgranule is almost spherical granule, have the particle diameter of 10 to 1000 microns and be made up of the simethicone of wax and 5 ~ 30%, described simethicone has the viscosity of 10 ~ 500000 centipoises.
2. Wax particles according to claim 1, is characterized in that described wax is selected from Cera Flava, Cera Chinensis, spermaceti, haze tallow, palm wax, refined paraffin wax, microwax, rice bran wax, sugarcane wax or glyceryl monostearate.
3. prepare a method for wax microgranule as claimed in claim 1, it is characterized in that: said method comprising the steps of:
1) simethicone of the wax of 1% ~ 90% mass fraction and 10 ~ 99% mass fractions is mixed and heated to the temperature of 70 DEG C ~ 150 DEG C;
2) under the rotating speed of 20 ~ 350 revs/min, this mixture is stirred to being uniformly dispersed;
3) continuous stirring 5 ~ 60 minutes at maintenance temperature;
4) under the condition stirred, cooling makes mixture solidify;
5) by simethicone unnecessary for gained mixture filtering and removing, thus wax microgranule is obtained.
4. method according to claim 3, is characterized in that in step 1) in, wax and simethicone are heated to the temperature range of 80 ~ 130 DEG C.
5. method according to claim 3, is characterized in that in step 1) in, wax and simethicone are heated to the temperature range of 90 ~ 120 DEG C.
6. method according to claim 3, is characterized in that in step 2) in, make the mixture of wax and simethicone carry out disperseing until be uniformly dispersed under 40 ~ 300 revs/min of ranges of speeds.
7. method according to claim 3, is characterized in that in step 2) in, make the mixture of wax and simethicone carry out disperseing until be uniformly dispersed under 50 ~ 200 revs/min of ranges of speeds.
8. method according to claim 3, is characterized in that in step 3) in, by the mixture continuous stirring 10 ~ 40 minutes of wax and simethicone.
9. method according to claim 3, is characterized in that in step 3) in, by the mixture continuous stirring 15 ~ 30 minutes of wax and simethicone.
10. method according to claim 3, is characterized in that in step 4) in, the mixture of wax and simethicone is cooled to less than 40 DEG C.
11. methods according to claim 3, is characterized in that in step 4) in, by the mixture cool to room temperature of wax and simethicone.
12. methods according to claim 3, is characterized in that in step 5) in, remove unnecessary simethicone by the mode of natural filtration, vacuum filtration or centrifugal filtration.
The purposes in cosmetics prepared by 13. wax microgranules according to claim 1.
The purposes in cleansing milk, cleansing cream, massage oil, massage cream prepared by 14. wax microgranules according to claim 1.
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| FR2815847B1 (en) * | 2000-10-27 | 2002-12-13 | Oreal | COSMETIC COMPOSITION COMPRISING FIBERS AND WAX |
| US20050260151A1 (en) * | 2002-09-06 | 2005-11-24 | Societe L'oreal, S.A. | Charging/separating cosmetic makeup compositions for keratin fibers |
| US7993632B2 (en) * | 2002-12-20 | 2011-08-09 | L'oreal S.A. | Composition for coating keratin fibres having a threading nature |
| JP4795245B2 (en) * | 2003-10-27 | 2011-10-19 | ユニリーバー・ナームローゼ・ベンノートシヤープ | Hair care composition |
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| DE102008021007A1 (en) * | 2008-04-25 | 2009-11-12 | Byk-Chemie Gmbh | Dispersions of waxes and inorganic nanoparticles and their use |
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Effective date of registration: 20171121 Address after: 100176 Building No. 9, No. 26, West Ring Road, West Ring Road, Beijing economic and Technological Development Zone, Daxing District, Beijing Co-patentee after: Beijing Xian Ren Tang beauty Technology Co., Ltd. Patentee after: Beijing Rongxiang Institute of Regenerative Medicine Co., Ltd. Address before: 100176 Building No. 9, No. 26, West Ring Road, West Ring Road, Beijing economic and Technological Development Zone, Daxing District, Beijing Patentee before: Beijing Rongxiang Institute of Regenerative Medicine Co., Ltd. |