CN106280569A - Black sphere pigments used for cosmetic and preparation method thereof - Google Patents

Black sphere pigments used for cosmetic and preparation method thereof Download PDF

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Publication number
CN106280569A
CN106280569A CN201610653810.6A CN201610653810A CN106280569A CN 106280569 A CN106280569 A CN 106280569A CN 201610653810 A CN201610653810 A CN 201610653810A CN 106280569 A CN106280569 A CN 106280569A
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suspension
cosmetic
sno
spherical sio
spherical
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Inventor
余慧忠
林正交
甘蓉芳
章梦令
熊小寒
林敏立
韦贝佩
周扬
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GUANGXI CHESIR PEARL EFFECT MATERIAL Co Ltd
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GUANGXI CHESIR PEARL EFFECT MATERIAL Co Ltd
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Publication of CN106280569A publication Critical patent/CN106280569A/en
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241—Containing particulates characterized by their shape and/or structure
    • A61K8/025—Explicitly spheroidal or spherical shape
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26—Aluminium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C09C3/063—Coating
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/12—Treatment with organosilicon compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10—General cosmetic use
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41—Particular ingredients further characterized by their size
    • A61K2800/412—Microsized, i.e. having sizes between 0.1 and 100 microns
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/42—Colour properties
    • A61K2800/43—Pigments; Dyes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/10—Interference pigments characterized by the core material
    • C09C2200/1004—Interference pigments characterized by the core material the core comprising at least one inorganic oxide, e.g. Al2O3, TiO2 or SiO2
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C2200/00—Compositional and structural details of pigments exhibiting interference colours
    • C09C2200/20—Interference pigments comprising a layer with a concentration gradient or a gradient of the refractive index
    • C09C2200/205—Interference pigments comprising a layer with a concentration gradient or a gradient of the refractive index of coloured inorganic materials

Abstract

The present invention relates to a kind of black sphere pigments used for cosmetic and preparation method thereof, it is with mean diameter D50It is 1 μm～the spherical SiO of 10 μm2As base material, at least it is coated with SnO on the surface of described base material2、Fe3O4Coating；Wherein, that contact with described substrate surface is SnO2；Specifically include spherical SiO2Make suspension, be then sequentially added into SnCl4, reproducibility auxiliary agent, FeSO4、AlCl3And the one in dimethicone or sodium silicate or coupling agent, eventually pass filter, be dried and prepare.The product that the present invention prepares has that the sticky sense of skin is low, skinfeel is splendid, pro-skin effect clear advantage, and has the spherical functional pigment of black of covering power, fading effect so that it is be widely used in cosmetics, particularly in eye cream, eye shadow.

Description

Black sphere pigments used for cosmetic and preparation method thereof
Technical field
The invention belongs to fine chemistry industry Material Field, be specifically related to a kind of black sphere pigments used for cosmetic and preparation side thereof Method.
Background technology
At present, the base material that major part pearlescent pigment is used mostly is the lamella base materials such as mica sheet, and a lot of oxides can It is deposited on its surface and embodies the pearl effect of uniqueness, but used due to pearlescent pigment is all that (its particle diameter all exists big particle diameter More than 10 μm) natural mica granule is made as pigment substrate, and the surface coating layer of this kind of base material is mostly and divides in island The Nano titanium dioxide of cloth, therefore in cosmetic field is applied, its skinfeel is poor, fine and smooth not.
In the research process that pigment performance is modified, although the biggest reason of pigment performance difference is from its pigment base The kind of material, but the most but rarely have lamella base materials such as giving up mica sheet and select the base material of other shapes, especially Carrying out, as pigment base material, the research being correlated with using ball shape granule, it is primarily due to, using spheroidal particle as base material system Techniques below problem is there is: when being coated with on spherical base material top layer, it is difficult to by other metal oxygens during standby pigment Up, even if cladding is up, it is also susceptible to obscission to compound cladding later, thus causes spherical base material coating metal oxygen Conversion ratio is low, be coated with the problems such as uneven, color benefit is poor for compound cladding.
Summary of the invention
The invention provides a kind of black sphere pigments used for cosmetic and preparation method thereof, thus solve in the past with Muscovitum The pigment skinfeel that the lamella base materials such as sheet prepare is poor, oil absorption high, and prior art is preparing face using spheroidal particle as base material During material, conversion ratio is low, be coated with the problems such as uneven, color benefit is poor to there is substrate surface metal-oxide cladding.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
With mean diameter D50It is 1 μm～the spherical SiO of 10 μm2As base material, at least it is coated with SnO on the surface of described base material2、 Fe3O4Coating；Wherein, that contact with described substrate surface is SnO2。
In technique scheme, more specifically technical scheme it may also is that in described coating, SnO2Clad ratio be 1%～ 5%, Fe3O4Clad ratio be 2%～20%.
Further: the coating being coated with successively on described spherical substrate surface is the one in A or B；Wherein, A is SnO2、 Fe3O4、Al2O3；B is SnO2、Fe3O4、Al2O3、SiO2；
The preparation method that its employing comprises the following steps:
A. by mean diameter D50It is 1 μm～the spherical SiO of 10 μm2Put in deionized water, prepare the Ith suspension；
The most under agitation, spherical SiO will first be accounted for2The SnCl of quality≤2%4Join in the Ith suspension, to this suspension In spherical SiO2Carry out cladding process；Then FeSO is added4, to having carried out SnCl4The spherical SiO that cladding processes2Again Secondary carry out cladding process so that it is reach black form and aspect, obtain the IIth suspension；
The most under agitation, spherical SiO will first be accounted for2The AlCl of quality 0%～5%3Add the IIth suspension, be initially charged account for spherical SiO2The AlCl of quality 0%～5%3, then add and account for spherical SiO2The dimethicone of quality 0%～5% or sodium silicate or coupling One in agent, obtains the IIIth suspension；
D. the IIIth suspension filtered, be dried.
In technique scheme, more specifically technical scheme is it may also is that the leading of deionized water that use in described step A Electricity rate is less than 20 μ S/cm.
Further: in described step B, adding FeSO4It is initially charged before solution and accounts for spherical SiO2The reduction of quality 0.5% Property auxiliary agent.
Owing to using technique scheme, the present invention obtains providing the benefit that:
1. due to the fact that employing mean diameter D50 be the spherical sio2 of 1 μm～10 μm as base material, and at described base material Surface is at least coated with SnO on the surface of described base material2、Fe3O4Coating, and that contact with described substrate surface is SnO2, and Make SnO2Clad ratio be 1%～5%, Fe3O4Clad ratio be 2%～20%, thus obtain that the sticky sense of skin is low, skinfeel is splendid, close Skin effect is obvious, and has the spherical functional pigment of black of covering power, fading effect so that it is be widely used in cosmetics, especially It is in eye cream, eye shadow.
2. the present invention is by preparation process, is initially charged SnCl4Carry out pretreatment, make spherical SiO2On the surface of base material It is coated with SnO2, it is coated with other metal-oxide and other material the most again, thus solves in the past at spherical base material table When being coated with on Ceng, it is difficult to by other metal-oxides cladding up, even if cladding is up, it is also susceptible to come off later Phenomenon, thus conversion ratio is low, be coated with the problems such as uneven, color benefit is poor to cause spherical base material coating metal oxide cladding.
3. deionized water conductivity is limited to less than 20 μ S/cm by the present invention, can effectively improve metal-oxide Hydrolysis, covered effect.
4. the present invention is by adding SnCl4Afterwards, FeSO is added4Front addition reproducibility auxiliary agent, such that it is able to effectively prevent FeSO4Ferrous ion in solution aoxidizes, and improves the covered effect of ferrum oxide, it is ensured that it is without obscission.
5. the present invention is by adding AlCl3, dimethicone or sodium silicate or coupling agent and control its consumption, effectively Promote the hydrophilic and oleophilic effect of pigment, improve its dispersibility etc. so that it is the application in cosmetics, particularly eye cream, eye shadow.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the pigment top layer coating particle characterization that comparative example prepares.
Fig. 2 is the SEM figure of the pigment top layer coating particle characterization that the embodiment of the present invention 1 prepares.
Fig. 3 is the SEM figure of the pigment top layer coating particle characterization that the embodiment of the present invention 2 prepares.
Fig. 4 is the SEM figure of the pigment top layer coating particle characterization that the embodiment of the present invention 3 prepares.
Detailed description of the invention
In order to better illustrate the present invention, below in conjunction with specific embodiment, the invention will be further described, and the present invention Protection domain be not intended to be limited to following example.
Wherein, the water conductivity of the deionized water involved by described embodiment 1-embodiment 4 is less than 20 μ S/cm.
The preparation method of comparative example black sphere pigments
A. the spherical SiO that 100g mean diameter is 5 μm is weighed2Put in the reactor that volume is 2L, add 1000ml go from Sub-water, stirring is allowed to dispersed formation suspension, prepares the Ith suspension；
B. the Ith suspension is warming up to 70 DEG C, with 20% sodium hydroxide the acid-base value of this suspension regulated to pH value be 9.0, so After constant temperature stir under add 0.7mol/L FeSO4Solution is until the color of described suspension becomes black form and aspect, and in this mistake Journey drips 20% sodium hydroxide to keep pH value constant；After the interpolation of described solution terminates, continue constant temperature and stir 20 minutes, To the IIth suspension；
C. FeSO is worked as4After solution adds, keep temperature and pH value constant, add 20ml 0.5mol/l AlCl3 Solution, and at this During drip 20% sodium hydroxide to keep pH value constant；After the interpolation of described solution terminates, continue constant temperature and stir 20 minutes, Obtain the IIIth suspension；
D. AlCl is worked as3 After solution adds, the IIIth suspension is continued constant temperature and stirs 20 minutes, then filter, at 80 DEG C of vacuum Dry.
This comparative example has prepared a kind of with mean diameter D50It it is the spherical SiO of 5 μm2As base material, this substrate surface is successively It is coated with Fe2O3、Al2O3The black sphere pigments of coating.
The preparation method of embodiment 1 black used for cosmetic sphere pigments
It comprises the following steps:
A. by 100g mean diameter D50It it is the spherical SiO of 1 μm2Put in deionized water, prepare the Ith suspension；
B. the Ith suspension is warming up to 65 DEG C, and dilute hydrochloric acid to regulate the acid-base value of this suspension to pH value be 1.5, then exist Constant temperature stirring is lower adds 200ml 0.5wt%SnCl4·5H2O solution, and drip 20% sodium hydroxide in the process to keep pH It is worth constant；As described SnCl4·5H2After the interpolation of O solution terminates, continue constant temperature and stir 15 minutes, obtain the IIth suspension；
C. the IIth suspension is warming up to 70 DEG C, and with 20% sodium hydroxide the acid-base value of this suspension regulated to pH value be 8, Then under constant temperature stirs, add 0.7mol/L FeSO4Solution is until the color of this suspension becomes black form and aspect, and in this mistake Journey drips 20% sodium hydroxide to keep pH value constant, obtain the IIIth suspension；
D. FeSO is worked as4After solution adds, keep temperature and pH value constant, continue the acid of the IIIth suspension with 20% sodium hydroxide Basicity regulation is 7 to pH value, then adds 15ml coupling agent under constant temperature stirring condition, and drips 20% hydrogen-oxygen in the process Changing sodium keeps pH value constant, obtains the IVth suspension；
E., after coupling agent adds, the IVth suspension is continued constant temperature at 75 DEG C and stirs 15 minutes, then obtained is hanged Dry at supernatant liquid filtration, 80 DEG C of vacuum.
The present embodiment has prepared a kind of with mean diameter D50It it is the spherical SiO of 1 μm2As base material, this substrate surface covers Coating be followed successively by SnO2、Fe3O4, and SnO in this coating2Clad ratio be 2%, Fe3O4The black that clad ratio is 12% spherical Pigment.
The preparation method of embodiment 2 black used for cosmetic sphere pigments
It comprises the following steps:
A. by 100g mean diameter D50It it is the spherical SiO of 10 μm2Put in deionized water, prepare the Ith suspension；
B. the Ith suspension is warming up to 65 DEG C, and dilute hydrochloric acid to regulate the acid-base value of this suspension to pH value be 1.0, then exist Constant temperature stirring is lower adds 400ml 0.5wt%SnCl4·5H2O solution, and drip 20% sodium hydroxide in the process to keep pH It is worth constant；As described SnCl4·5H2After the interpolation of O solution terminates, add the sodium hydrosulfite of 0.4g, continue constant temperature and stir 20 minutes, To the IIth suspension；
C. the IIth suspension is warming up to 70 DEG C, and with 20% sodium hydroxide by the acid-base value regulation of this suspension to pH value is 8.5, under constant temperature stirs, then add 0.7mol/L FeSO4Solution until the color of this suspension becomes black form and aspect, and Drip 20% sodium hydroxide during this to keep pH value constant, obtain the IIIth suspension；
D. as described FeSO4After solution interpolation terminates, keep the temperature of the IIIth suspension and pH value constant, be then initially charged spherical 30ml 0.5mol/l AlCl3Solution, is added followed by 3g coupling agent, and drips 20% sodium hydroxide in the process and keep PH value is constant, obtains the IVth suspension；
E., after coupling agent adds, the IVth suspension is continued constant temperature and stirs 20 minutes, then dry at filtration, 80 DEG C of vacuum.
The present embodiment has prepared a kind of with mean diameter D50It it is the spherical SiO of 1 μm2As base material, this spherical SiO2Base material It is coated with SnO successively2、Fe3O4、Al2O3SnO in coating, and this coating2Clad ratio be 2.4%, Fe3O4Clad ratio be 14%, Al2O3The black sphere pigments that clad ratio is 2.4%.
The preparation method of embodiment 3 black used for cosmetic sphere pigments
It comprises the following steps:
A. by 80g mean diameter D50It it is the spherical SiO of 5 μm2Put in deionized water, prepare the Ith suspension；
B. prepared Ith suspension is warming up to 68 DEG C, and the value acid-base value of this suspension is regulated to pH value 1.2, so by dilute hydrochloric acid After constant temperature stir under add 300ml 0.5wt%SnCl4·5H2O solution, and drip 20% sodium hydroxide in the process and protect Hold pH value constant；As described SnCl4·5H2After the interpolation of O solution terminates, add 0.4g carbamide, continue constant temperature and stir 30 minutes, To the IIth suspension；
C. the IIth suspension is warming up to 80 DEG C, and with 20% sodium hydroxide, the value acid-base value of this suspension is regulated to pH value 9, Then under constant temperature stirs, add 0.7mol/L FeSO4Solution is until the color of this suspension becomes black form and aspect, and in this mistake Journey drips 20% sodium hydroxide to keep pH value constant, obtain the IIIth suspension；
D. as described FeSO4After solution adds, keep the temperature of the IIIth suspension and pH value constant, be then initially charged 65ml 0.5mol/l AlCl3Solution, is added followed by 50ml 0.5mol/l sodium silicate, and drips 20% sodium hydroxide in the process Keep pH value constant, obtain the IVth suspension；
E., after sodium silicate adds, the IVth suspension is continued constant temperature and stirs 30 minutes, then dry at filtration, 80 DEG C of vacuum.
The present embodiment has prepared a kind of with mean diameter D50It it is the spherical SiO of 1 μm2As base material, this substrate surface is successively It is coated with SnO2、Fe3O4、Al2O3、SiO2, and SnO in this coating2Clad ratio be 3%, Fe3O4Clad ratio be 9%, Al2O3's Clad ratio is 3%, SiO2The black sphere pigments that clad ratio is 1.2%.
Performance detects
One, the detection of oil absorption
1. detection method: accurately weigh sample 1.0～1.5g, be accurate to 0.0001g, as on flat board, drips with glue head dropper Refined oleum lini, sample-adding must not exceed 10 every time, grinds by toolsetting pressure after adding, and makes oil penetrate into given the test agent, continues with this speed Till degree drops to oil and sample formation agglomerate.From that point on, needing to be fully ground with toolsetting after often adding one, when being formed, denseness is equal Even paste, does not the most split the most broken, when can stick on flat board again, is terminal.
Oil absorption oil quality needed for every 100g product represents, calculation is as follows:
m%= M/m * 100%
In formula: the consumption of M-expression oleum lini, g；
The quality of m-sample, g.
2. testing result: be shown in Table 1.
Table 1
As can be seen from the above Table 1, the oil absorption of pigment that embodiment 1～3 prepares is relatively low.
Two, pigment top layer characterizes coating particle characterization
Can be seen that from Fig. 1 to Fig. 4, although the granules of pigments in comparative example is the most spherical in shape, but its granular size is uneven, and its The coating shedding phenomenon on top layer is serious；And the granules of pigments of embodiment 1-3 is spherical, and being evenly distributed, the coating on its top layer does not has There is break-off.

Claims (6)

1. a black sphere pigments used for cosmetic, it is characterised in that: with mean diameter D50It is 1 μm～the spherical SiO of 10 μm2Make For base material, at least it is coated with SnO on the surface of described base material2、Fe3O4Coating；Wherein, with described substrate surface contacts it is SnO2。
Black sphere pigments used for cosmetic the most according to claim 1, it is characterised in that: in described coating, SnO2Cladding Rate is 1%～5%, Fe3O4Clad ratio be 2%～20%.
Black sphere pigments used for cosmetic the most according to claim 1 and 2, it is characterised in that: described spherical substrate surface On the coating that is coated with successively be the one in A or B；Wherein, A is SnO2、Fe3O4、Al2O3；B is SnO2、 Fe3O4、Al2O3、 SiO2。
4. the preparation method of a black sphere pigments used for cosmetic, it is characterised in that comprise the following steps:
A. by mean diameter D50It is 1 μm～the spherical SiO of 10 μm2Put in deionized water, prepare the Ith suspension；
The most under agitation, spherical SiO will first be accounted for2The SnCl of quality≤2%4Join in the Ith suspension, in this suspension Spherical SiO2Carry out cladding process；Then FeSO is added4, to having carried out SnCl4The spherical SiO that cladding processes2Again Carry out cladding process, until it reaches black form and aspect, obtain the IIth suspension；
The most under agitation, spherical SiO will first be accounted for2The AlCl of quality 0%～5%3Add the IIth suspension, then add and account for Spherical SiO2One in the dimethicone of quality 0%～10% or sodium silicate or coupling agent obtains the IIIth suspension；
D. the IIIth suspension filtered, be dried.
The preparation method of black sphere pigments used for cosmetic the most according to claim 4, it is characterised in that: described step A The conductivity of the deionized water of middle use is less than 20 μ S/cm.
6. according to the preparation method of the black sphere pigments used for cosmetic described in claim 4 or 5, it is characterised in that: described B walks In Zhou, adding FeSO4It is initially charged before solution and accounts for spherical SiO2The reproducibility auxiliary agent of quality 0.5%.
CN201610653810.6A 2016-08-11 2016-08-11 Black sphere pigments used for cosmetic and preparation method thereof Pending CN106280569A (en)

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Application publication date: 20170104