The best mode that carries out an invention
Cosmetics of the present invention are characterised in that: contain four (trimethylsiloxy group) silane shown in the following chemical formula (1),
[(CH
3)
3SiO]
4Si (1)。
M4Q is a chemical inertness, and excellent in safety.In addition, can not make skin have the peculiar dry sensation of annular siloxane, the sensation excellence when smearing.
The boiling point of M4Q under normal pressure is 222 ℃.Than boiling point under the normal pressure be 190 ℃ M3T volatilization slowly.Viscosity under the room temperature is 3.1mm
2About/s.Among the present invention, " volatility " be meant under 1 atmospheric pressure, the volatility 25 ℃ the time.M4Q can be blended in arbitrarily in the scope of 0.1-90 quality % in the cosmetics, preferably by with other composition combination and according to dosage form, is adjusted to suitable melting concn.The amount of M4Q is lower than above-mentioned lower limit, then can not bring into play the advantage of M4Q, and surpasses above-mentioned higher limit, and the too high tendency of oiliness sense is then arranged.
By M4Q is mixed with M3T, can make and have desirable volatility, when being used for skin, make skin have the cosmetics of more refreshing sensation.The combined amount of M4Q and M3T is than can suitably regulating according to the form of cosmetics, desirable boiling characteristics, preferably 5: 95-90: mix in the scope of 10 (quality %).If in this scope, mix, then not only can be adjusted to desirable volatility, desirable oiliness sense can also be regulated, and the high cosmetics of stability can be obtained.For example making up bottoming (down) material can be according to 60: 40-40: 60 mix.
The total combined amount of preferred M4Q and M3T is with respect to the scope of cosmetics total amount at 0.1-90 quality %, more preferably in the scope of 0.5-60 quality %.As long as in this scope, user just can actually be experienced the suitable volatility of regulating by M4Q and M3T.
Except that M3T, by volatile all kinds of solvents is used in combination with M4Q,, can reduce the oiliness sense of M4Q regulating desirable volatile while, can prepare the cosmetics of smearing sense with salubrious sensation.The combination, particularly ethanol of lower alcohols such as for example preferred and ethanol, isopropyl alcohol by with the azeotropic effect of M4Q, can produce salubrious sensation.
On the other hand, preferred mix be selected from Fancol ID, isodecane, 2-Methylpentadecane, isoparaffin, straight chain shape volatile siloxane, terpenic one or more.Particularly the evaporation rate of Fancol ID, isodecane, 2-Methylpentadecane is fast, with the M4Q combination, can make sustainable evaporable dosage form.Fancol ID, isodecane, 2-Methylpentadecane stop up on skin, and the skin irritant problem of generation is then arranged, and therefore preferably improve on prescription, make the property stopped up minimizing.Preferred above-mentioned each volatile solvent and M4Q, as required, the mass ratio of the mixture of M4Q and M3T is 10: 90-90: use in 10 the scope.
Volatile siloxane commonly used is used with M4Q, can control evaporation rate or change organoleptic attribute.The example of above-mentioned volatile siloxane commonly used has: cyclic dimethyl polysiloxane that the metric silicon atom number of limit that can not produce dry sensation is 4-6 and silicon atom number are 4 or 5 straight chain dimethyl polysiloxane.The example of above-mentioned cyclic dimethyl polysiloxane has: octamethylcy-clotetrasiloxane, decamethylcyclopentaandoxane, ten diformazan basic rings, six siloxanes etc., their combined amount is identical with above-mentioned volatile solvent.
For example be used in combination emulsifying agent, during the preparation emulsified make-up, above-mentioned M4Q can bring stable in time this high emulsified make-up.Emulsified make-up has O/W type and w/o type, can suitably select wherein any form according to the purposes of cosmetics and the amount of blended oil preparation etc.Used emulsifying agent can mix the nonionic silicone type surface active agent, side chain silicone-type polyglyceryl modified siloxane for example, side chain silicone-type polyether modified siloxane, alkyl, polyether is modified siloxane altogether, polyether modified siloxane, cross-linking type polyglyceryl modified siloxane, the sugar modified siloxane, one or more of glyceryl modified siloxane are preferably selected from side chain silicone-type polyglyceryl modified siloxane especially, side chain silicone-type polyether modified siloxane, alkyl, polyether is modified siloxane altogether, polyether modified siloxane, one or more of cross-linking type polyglyceryl modified siloxane.The compatibility excellence of these compositions and volatile siloxane of the present invention helps forming stable emulsion.In these emulsifying agents, the HLB value by 6 or following be the particularly preferred combination of preparation w/o type emulsification cosmetic.Also can be by being used in combination with other emulsifying agent, the HLB value that makes emulsifying agent integral body be 6 or below.With respect to the total amount of cosmetics, mentioned emulsifier is preferably at 0.05-20 quality %, more preferably use in the scope of 0.1-10 quality %.The particular content of these chemical compounds for example is recorded in TOHKEMY 2002-179548 number, TOHKEMY 2002-179797 number, TOHKEMY 2002-179798 number, TOHKEMY 2002-154917 number, Japanese kokai publication hei 7-252122 number, Japanese kokai publication hei 9-175928 number, Japanese Patent Publication 44-4679 number, Japanese kokai publication sho 57-14797 number, Japanese kokai publication sho 55-18424 number, Japanese kokai publication hei 10-182354 number, TOHKEMY 2001-2555 number, TOHKEMY 2000-63233 number, Japanese kokai publication hei 6-145023 number, Japanese kokai publication hei 7-187945 number, Japanese kokai publication hei 5-112424 number, in the Japanese kokai publication hei 9-71504 number communique such as grade etc.
M4Q dissolubility excellence for example can high concentration be dissolved various siloxane-based material commonly used in the cosmetics.As siloxane-based material, preferably modified siloxane, siliconization プ Le ラ Application, the ester modified siloxanes of ammonia, alkyl-modified siloxanes etc. are used in combination altogether with silicone resin, silicone-modified organic bond, fluorine modified siloxane resin, polyamide modified siloxanes, acrylated siloxanes, alkyl acrylic.These siloxane-based materials can be dissolved in the past the low viscosity dimethyl polysiloxane or annular siloxane etc. in use, but M4Q can dissolve these materials with higher concentration, the result can reduce the amount of taking composition out of, has the advantage that can improve the prescription degree of freedom.In the cosmetics, these resinous principles preferably use in the 0.3-20 quality % scope with respect to the cosmetics total amount.As long as in this scope, just can obtain to bring into play the characteristic of silicone resin, the preparation of cosmetic persistence excellence.These chemical compounds are when carrying out silicone compounds that modification obtains by various modification groups to siloxane chain or silicone resin, and its particular content is recorded in Japanese kokai publication sho 61-161211 number, Japanese kokai publication hei 4-312511 number, Japanese kokai publication hei 2-42008 number, Japanese kokai publication hei 9-25218 number, TOHKEMY 2003-55155 number, Japanese kokai publication sho 59-20360 number, Japanese kokai publication hei 9-110633 number, Japanese kokai publication hei 6-9332 number, Japanese kokai publication hei 10-29921 number, No. the 2708199th, French Patent (FRP), Japanese kokai publication hei 3-264510 number, Japanese kokai publication hei 4-66513 number, Japanese kokai publication hei 5-262987 number, wait communique etc. Japanese kokai publication hei 5-194147 number.
The dissolubility of the excellence of above-mentioned M4Q is fit to the dissolving oily dirt.That is the M4Q abluent purposes that is suitable as the cleaning agent of removing oil-based cosmetic preparation and removes the sebum dirt.In the preferred embodiments of the invention, cleaning agent contains M4Q and nonionic is a surfactant.M4Q preferably is the scope mixing of 1-50 quality % with the total amount with respect to cleaning agent.As long as in this scope, then can show the ability of effectively cleaning.
Nonionic is a surfactant so long as the material that adopts usually in the cosmetics can use.The particularly compatibility excellence of silicone type surface active agent and M4Q, thereby preferred the use.The example of silicone type surface active agent has: the modification group that has the alkyl, alcohol hydroxyl group, phenyl, glyceryl, polyglyceryl, sugared modification Ji, oxazolinyl, PFPE etc. of at least a carbon number 2-30 that is selected from polyoxyalkylenes, can be replaced by atomic components such as fluorine for the dimethyl polysiloxane chain, and have the modification group with the form of side group, terminal groups or block unit, wherein a kind of modification group in back serve as must the formation unit with hydrophilic groups such as polyoxyalkylenes, glyceryl, polyglyceryl, sugared modification base, holo-fluorine polyester, alcohol hydroxyl groups.
For example have: polyether-modified organopolysiloxane (another name: polyoxyalkylene modified siloxane or polyether modified siloxane), alkyl polyoxyalkylene altogether modified siloxane (another name: polyoxyalkylene alkyl is modified siloxane altogether), fluoridize dimethyl silica alkanol, perfluoroalkyl polyoxyalkylene modified siloxane, perfluoro alkoxy polyoxyalkylene modified siloxane, glyceryl modified siloxane, polyglyceryl modified siloxane, perfluoroalkyl polyglyceryl modified siloxane, glycosyl modified siloxane etc. altogether altogether altogether.The example of above-mentioned polyether-modified organopolysiloxane has KF351, KF6011, KF6012, KF6015, KF6017, KF6026, FPD6131 of chemical industry society of SHIN-ETSU HANTOTAI system etc.
Can preferably use sorbitan fatty acid ester, fatty acid glyceride, polyglyceryl fatty acid ester, methyl glycol fatty acid ester, cithrol, sucrose fatty acid ester, polyoxyethylene alkyl ether, the polyoxypropylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene fatty acid ester, the polyoxyethylene sorbitan fatty acid ester, Polyoxyethylene Sorbitol Fatty Acid Esters, the polyoxyethylene fatty acid glyceride, the polyoxyethylene methyl glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated Oleum Ricini, polyoxyethylene phytostanol ether, polyoxyethylene plant sterol ether, polyoxyethylene cholestane alcohol ether, polyoxyethylene cholesterol ether, alkanolamide, sugar ether, nonionics such as sugar amide are surfactant.This nonionic be the combined amount of surfactant with respect to the preferred 0.1-25 quality of the total amount of cleaning agent %, preferred especially 0.5-10 quality %.
When this cleaning agent and water are mixed and made into oil-in-water type, preferred O/W type, in this case, use HLB value be 10 or the above above-mentioned nonionic of conduct be surfactant, then have the ability of effectively cleaning, thereby preferably.
This cleaning agent is mixing water not also.When being the oil type cleaning agent of not mixing water,, can make the preparation of transparent type by regulating the refractive index of oil preparation.
That the form of this cleaning agent has is liquid, spray shape, scraps of paper shape, vaporific, mousse etc., has facial, circumference of eyes to use etc. with, hair, whole body.
Then, abluent is described.Abluent is even without the place of washing equipment and be used to remove the dirt of skin, scalp and (the Japanese kokai publication hei 5-201851 communique) of cosmetics.In the past, for realizing this purposes use annular siloxane.But as stating before, annular siloxane produces the dry sensation of the skin that is called as dry sensation, dissolves the weak problem of sebum composition ability in addition.Relative therewith, M4Q can make and not produce dry sensation, and sebum dissolving power height can not produce stimulation and obstacle to skin, have the abluent of good usability.
The preferred embodiments of the invention are: the skin abluent contains M4Q and methyl phenyl silicone.This methyl phenyl silicone can make and apply some make up usually employedly, preferably is liquid under room temperature, normal pressure.Preferred this methyl phenyl silicone uses in 0.5-25 quality % scope with respect to the total amount of abluent.As long as in this scope, use abluent after the oiliness sense few, can make sensation better.
This abluent boiling point under normal pressure is below 225 ℃, preferably further contains under 1 atmospheric pressure, 25 ℃ to have volatile solvent.This volatile solvent has volatile siloxanes such as aforesaid methyl three (trimethylsiloxy group) silane, annular siloxane, straight chain low molecular weight polyorganosiloxane, lower alcohols such as ethanol, isopropyl alcohol, propanol, liquid paraffin,lights such as Fancol ID etc.Wherein methyl three (trimethylsiloxy group) silane, alcoholic acid safe with the compatibility excellence of sebum composition, preferably mixes.In addition also can mixing water, but might make sebum or dirt be attached to skin again, therefore preferred combined amount does not preferably contain especially at 10 quality % or following of abluent total amount.Abluent composed as follows: with respect to the total amount of abluent, M4Q is 5-70 quality %, and methyl phenyl silicone is 0.5-25 quality %, and volatile solvent is 25-94.5 quality %, can improve clean effect like this.
The concrete purposes of this abluent has: cleaning agent, do (De ラ イ) shampoo, that its form is fit to adopt is liquid, spray shape, scraps of paper shape.
M4Q is to dispersing of pigments ability height, and the disperse medium that is suitable as in the cosmetics that contain pigment mixes.This purposes was to adopt ester oil or annular siloxane in the past, made the pigment dispersed slurry of dividing by color that is called as the mill base mode in advance, came the color of brewed product by their combination.The advantage of this method is that toning is than being easier to.But the ester oil mechanical energy when disperseing sometimes produces deterioration, causes abnormal flavour or variable color etc.On the other hand, annular siloxane is stable to mechanical force, but dispersion efficiency is poor, and pigment is difficult to homodisperse.And the present invention finds, M4Q is stable to mechanical activation comminution, and the dispersion efficiency height of coloring pigment, is suitable as dispersion solvent.Therefore various coloring pigments are disperseed, when being mixed in the cosmetics, find the chroma height of gained cosmetics, have bright-coloured tone.
Coloring pigment can use any pigment so long as use in the cosmetics.(spherical, bar-shaped, needle-like, tabular, amorphous, flakey, spindle shape etc.) or particle diameter (smoke-like, microgranule, pigment-level etc.), grain structure (porous, non-hole etc.) all can use no matter its shape.The example of colored pigment has: ferrum oxide, hydrated ferric oxide., inorganic red pigment such as iron titanate, inorganic brown series pigments such as gamma-iron oxide, iron oxide yellow, inorganic yellow series pigments such as loess, iron oxide black, low order acidify チ Application, inorganic black pigment such as carbon black, manganese violet, inorganic violet pigment such as cobalt violet, chromic oxide gel, chromium oxide, cobalt oxide, inorganic viridine green such as cobalt titanate, Prussian blue, inorganic blue series pigments such as ultramarine, with tar (-Le) is the pigment that pigment is made the color lake, natural pigment is made the pigment in color lake, and the synthetic resin powder that these powder are composited etc.The object lesson of tar colorant has red No. 3, red No. 104, red No. 106, red No. 201, red No. 202, red No. 204, red No. 205, red No. 220, red No. 226, red No. 227, red No. 228, red No. 230, red No. 401, red No. 505, yellow No. 4, yellow No. 5, yellow No. 202, yellow No. 203, yellow No. 204, yellow No. 401, blue No. 1, blue No. 2, blue No. 201, blue No. 404, green No. 3, green No. 201, green No. 204, green No. 205, orange No. 201, orange No. 203, orange No. 204, orange No. 206, orange No. 207 etc., natural colour have and is selected from carminic acid, laccaic acid, carthamin, brazilin, the pigment of crocin etc.Wherein, preferred tar colorant and color lake thereof, natural pigment.
These coloring pigments are for example preferably handled (preferred perfluoralkyl phosphate processing or perfluoroalkyl silane treatment by fluorine compounds; PFPE is handled; the fluoro siloxane treated; the fluorinated siloxane resin treatment); siloxane treated (handle by the preferable methyl hydrogen polysiloxanes; dimethyl polysiloxane is handled; vapor phase method tetramethyl tetrahydrochysene cyclotetrasiloxane is handled); silicone resin is handled (preferred trimethylsiloxy group silicic acid is handled); side group is handled methods such as (after the vapor phase method siloxane treated) addition alkyl chains; silane coupler is handled; titanium coupling agent is handled; silane treatment (preferred alkyl silane or alkyl silazane are handled); oil preparation is handled; N-acyl group lysine is handled; polyacrylic acid is handled; metallic soap is handled (preferred stearic acid or myristate); acrylic resin is handled; metal oxide treated; agar is handled; surface treatments such as DNA (deoxyribonucleic acid) processing are further preferably used a plurality of above-mentioned treatment combinations.Wherein, the surface treatment of the dispersing characteristic excellence due to the M4Q preferably has N
ε-lauroyl-L-lysine is handled, alkyl silane is handled, side group is handled, the N of preferred especially productive rate, cost-performance excellence
ε-lauroyl-L-lysine is handled, alkyl silane is handled.
M4Q combined amount in the dispersion liquid is a 20-90 quality % scope with respect to the gross mass of dispersion liquid preferably.In order to improve the dispersibility of coloring pigment, preferred combination is used surfactant, the preferred especially silicone type surface active agent that has with the M4Q similar structures that uses.The example of silicone type surface active agent has the modification group that has the alkyl, alcohol hydroxyl group, phenyl, glyceryl, polyglyceryl, sugared modification Ji, oxazolinyl, PFPE etc. of at least a carbon number 2-30 that is selected from polyoxyalkylenes, can be partly replaced for the dimethyl siloxane chain, and have the modification group with the form of side group, terminal groups or block unit, wherein a kind of modification group in back serve as must the formation unit with hydrophilic groups such as polyoxyalkylenes, glyceryl, polyglyceryl, sugared modification base, holo-fluorine polyester, alcohol hydroxyl groups.For example have: polyether-modified organopolysiloxane (another name: polyoxyalkylene modified siloxane or polyether modified siloxane), alkyl polyoxyalkylene altogether modified siloxane (another name: polyoxyalkylene alkyl is modified siloxane altogether), fluoridize dimethyl silica alkanol, perfluoroalkyl polyoxyalkylene modified siloxane, perfluoro alkoxy polyoxyalkylene modified siloxane, glyceryl modified siloxane, polyglyceryl modified siloxane, perfluoroalkyl polyglyceryl modified siloxane, glycosyl modified siloxane etc. altogether altogether altogether.The example of above-mentioned polyether-modified organopolysiloxane has KF6012, KF6015, KF6017, KF6026, FPD6131 of chemical industry society of SHIN-ETSU HANTOTAI system etc.The example of other dispersant preferably uses sorbitan fatty acid ester, fatty acid glyceride, polyglyceryl fatty acid ester, methyl glycol fatty acid ester, cithrol, sucrose fatty acid ester, polyoxyethylene alkyl ether, the polyoxypropylene alkyl ether, polyoxyethylene alkyl phenyl ether, polyoxyethylene fatty acid ester, the polyoxyethylene sorbitan fatty acid ester, Polyoxyethylene Sorbitol Fatty Acid Esters, the polyoxyethylene fatty acid glyceride, the polyoxyethylene methyl glycol fatty acid ester, polyoxyethylene castor oil, polyoxyethylene hydrogenated Oleum Ricini, polyoxyethylene phytostanol ether, polyoxyethylene plant sterol ether, polyoxyethylene cholestane alcohol ether, polyoxyethylene cholesterol ether, alkanolamide, sugar ether, nonionics such as sugar amide are surfactant.To be surfactant mix the scope of preferred especially 0.5-15 quality % with respect to the quality optimization of dispersion liquid to this nonionic with 0.1-20 quality %.
This dispersion liquid uses pulverizer that above-mentioned each composition is disperseed.After preferably pressing pigment making dispersion liquid,, be modulated into desirable color with multiple dispersion liquid appropriate combination.Process for dispersing has: wet type medium type pulverizer, roller mill, jet mill, ultrasonic grinding machine, the ア Le テ イ マ イ ザ-シ ス テ system methods such as high pressure impact grinder, dispersion machine, high speed homogenizer, homogenizer such as (ス ギ ノ マ シ Application corporate systems) of ball mill or マ イ Network ロ ス (nara machinery is made made) etc.Wherein, use wet type medium type pulverizer, the degree of grinding height, and can obtain stable dispersions, and the productive rate excellence, thereby preferred.Wet type medium type pulverizer can be vertical, also can be horizontal, and can be that continous way also can be a batch (-type).Use these devices,, also have according to circumstances dispersant, oil preparation to mix and pulverize M4Q and pigment.Pulverization conditions is relevant with the ability of each device, makes the pulverizing time, pulverizes the chart of number of times and mean diameter or color, and setting and making chart is the condition of steady statue, and this is effective for the stability of color of guaranteeing every batch.
M4Q has as the example of the suitable cosmetics of pigment disperse medium: beautification product, particularly lipstick, eyeliner, mascara, brow, eye shadow cream, nail polish paste, foundation cream, cover up apply some make up, チ-Network, hair dye etc.
Except that above-mentioned various pigment,, can obtain oil-based cosmetic preparation by mixing 25 ℃ of oily matters for solid-state or paste.In the past, in the oil-based cosmetic preparations such as known lipstick, in order to improve anti-chromatic effect or the raising persistence of moving, can mixed volatilization siloxanes (Japanese kokai publication hei 8-92036 communique, Japanese kokai publication hei 3-77162 communique, Japanese kokai publication hei 10-29915 communique).But as previously mentioned, volatile siloxane, particularly annular siloxane can give user with dry sensation when smearing and after crossing certain hour.Relative therewith, by using M4Q, not only can not produce dry sensation, to compare with above-mentioned annular siloxane, volatility is low, so excellent in stability in time, and therefore the pigment-dispersing excellence can obtain brightness, gloss excellence, the oil-based cosmetic preparation that chroma is high.
In the embodiment preferred of the present invention, oil-based cosmetic preparation contains M4Q, pigment, polybutene.Preferred M4Q with respect to the total amount of oil-based cosmetic preparation in 0.1-60 quality % scope, more preferably 1-50 quality % scope is used.So long as this scope can effectively obtain preparation stabilization, the anti-advantages such as chromatic effect, chroma raising of moving.
Pigment optimization uses in 0.1-50 quality % scope, further preferred 0.5-35 quality % scope with respect to the total amount of oil-based cosmetic preparation.So long as this scope just has the stability of formulation of guaranteeing, feel good advantage.
Preferred isobutene. of polybutene and n-butene copolymerization gained, further preferably have liquid at normal temperatures to paste.The preferred polybutene mean molecule quantity of described polybutene is in the 500-2700 scope, in the scope of further preferred 800-1200.Mean molecule quantity is less than 500, and then high-temperature stability has problem, if 2700 or more than, be clamminess the sense smarten, feel bad.
In order to improve stability, can carry out hydrogenation treatment to the polybutene that uses among the present invention, also can carry out refinement treatment.The combined amount of this polybutene is preferably 2-40 quality % with respect to the oil-based cosmetic preparation total amount.Less than 2 quality %, the slow-releasing of uncontrollable M4Q then, and surpass 40 quality %, the sense of then being clamminess strengthens, the sensation variation.
This oil-based cosmetic preparation can be by known method preparation in the past.For example can use roller, ball mill etc. to disperse mechanism to be equipped with, can also make mill base, it is mixed prepare with ball mill etc.M4Q is a volatile material, and container need use the container of closed.
This oil-based cosmetic preparation is suitable for lipstick, foundation cream, eye shadow cream, eyeliner, mascara, チ-Network, cover up apply some make up, sunscreen, cosmetic backing material etc.
Except that above-mentioned pigment and oily matter, by using surfactant, mix moisture can prepare solid-state beauty treatment and apply some make up.Among the present invention, the preferred version that beauty treatment applies some make up is as follows, and here, each combined amount is the amount with respect to the cosmetics gross mass.
(A) M4Q of 10-30 quality %,
(B) 5-10 quality % be selected from multivalence alcohol or saccharide a kind or above polyol compound,
(C) 1.5-3.5 quality % be selected from sorbitan fatty acid ester, polyglyceryl fatty acid ester, sucrose fatty acid ester, polyose alkylether a kind or above surfactant,
(D) 3-7 quality % 25 ℃ down for the oily matters of solid or paste,
(E) pigment of 30-45 quality % and
(F) pure water of 5-25 quality %.
(B) example of polyol compound has: glycols, polysaccharides etc. such as ethylene glycol, propylene glycol, butanediol, diethylene glycol, dipropylene glycol, glycerol, diglycerol, sorbitol, マ Le PVC ト-Le, trehalose, Raffinose, xylitol, mannitol, hyaluronic acid or its salt, trehalose derivant, Raffinose derivant, Polyethylene Glycol, polyglycereol.The example of trehalose derivant or Raffinose derivant has these sugared alkyl ether derivatives or alkenyl ether derivant, and preferred especially carbon number is the alkyl ether derivative of 1-24, the alkenyl ether derivant that carbon number is 3-24.Polysaccharide has: カ ラ ギ Na-Application, agar, more create glue, locust bean gum, Radix Acaciae senegalis, Tragacanth, pectin, xanthan gum, glucosan, cellulose etc.With respect to the solid-state beauty treatment total amount that applies some make up, mix this polyhydric alcohol with the scope of 5-10 quality %.The combined amount of polyhydric alcohol makes skin produce tight sense less than above-mentioned lower limit after then smearing, and surpasses above-mentioned higher limit, and the sense that then occurs being clamminess is not preferred.
(C) can use above-mentioned various surfactant in the Solic cosmetic of the present invention, but wherein from excellent in stability, can obtain good organoleptic consideration, the preferred use is selected from least a of anhydrous sorbitol isostearate, sorbitan monooleate.The total amount that the combined amount of this surfactant applies some make up with respect to solid-state beauty treatment is a 1.5-3.5 quality % scope.Combined amount is less than above-mentioned lower limit, the problem that then has resistance to water, anti-sebum to weaken; Surpass the above-mentioned restriction of going up, the problem that produces the sense of being clamminess is then arranged.
(D) oily matter of solid-state or paste is except the oil-based solvent or resinae that for example used in the cosmetics in the past, also comprises to be dissolved in other oil-based solvent, becomes resin, the binding agent class of paste at normal temperatures.Representational for example have: ホ ホ バ wax, Brazil wax, candelilla wax, rice bran wax, Lac, lanoline, Cera Flava, white beeswax, ceresine, ceresin, paraffin, microwax, vaseline, lauric acid, myristic acid, Palmic acid, stearic acid, mountain Yu acid, the 12-hydroxy stearic acid, 9-undecylenic acid, lauryl alcohol, myristyl alcohol, spermol, stearyl alcohol, oleyl alcohol, behenyl alcohol, batilol, .alpha.-hexadecylglyceryl ether, selachyl alcohol, iso stearyl glyceryl ether, ethyl stearte, butyl stearate, myristyl myristate, cetyl myristate, the myristic acid stearyl, the castor oil acid cetyl, three (9-undecylenic acid) glyceride, four myristic acid pentaerythritol esters, the lactic acid cetyl, hydroxy stearic acid octyl group ester, cholesteryl stearate, the isostearic acid cholesterol ester, the hydroxy stearic acid cholesterol ester, Cholesterol 3.beta.-oleate, oleic acid dihydrocholesterol ester, the isostearic acid plant sterol ester, Polyethylene Glycol, polyglycereol, Petiolus Trachycarpi oil, Oleum Cocois, Adeps Bovis seu Bubali, hydrogenated oil and fat, house oil, シ ア バ -, egg oil or polyethylene, polypropylene, politef, acrylic acid silica alkane, acrylate copolymer or its salt, acrylic acid methacrylic acid copolymer or its salt, resinaes such as polyvinylpyrrolidone.The combined amount of the oil preparation of this solid-state or paste is 3-7 quality % with respect to the cosmetics gross mass.Combined amount then is difficult to obtain resistance to water, anti-sebum less than above-mentioned lower limit, surpasses above-mentioned higher limit, then is difficult to remove cosmetics, the sensation variation.
(E) pigment mixes with 30-45 quality % with respect to the total amount of solid-state shape cosmetics.Combined amount is during less than above-mentioned lower limit, and the stability of cosmetics may be not enough, therefore preferably is used in combination with the oil-base gel agent, is made for above-mentioned lower limit or above cosmetics.On the other hand, if combined amount surpasses above-mentioned higher limit, then the sensation variation of cosmetics also is difficult to remove in addition.
Pigment can use any of hydrophilic pigment, hydrophobicity pigment so long as the employed pigment of common cosmetics gets final product, and especially preferably uses hydrophobicity pigment.Normally used pigment for example has inorganic powder, organic dust, surfactant metal salt powder, colored pigment, pearlescent pigment, metallic powdery pigment, natural pigment etc.
Described colored pigment before removing, tar colorant, outside the natural pigment, inorganic powder has the pigment-level titanium oxide, zirconium oxide, the pigment-level zinc oxide, cerium oxide, magnesium oxide, barium sulfate, calcium sulfate, magnesium sulfate, calcium carbonate, magnesium carbonate, Talcum, Muscovitum, Kaolin, sericite, white mica, synthetic mica, phlogopite, rubellan, biotite, lepidolite, silicic acid, silicic acid anhydride, aluminium silicate, magnesium silicate, Magnesiumaluminumsilicate, calcium silicates, barium silicate, strontium silicate, the wolframic acid slaine, hydroxyapatite, Vermiculitum, Ha イ ジ ラ イ ト, bentonite, Montmorillonitum, Strese Hofmann's hectorite., zeolite, ceramic powders, calcium hydrogen phosphate, aluminium oxide, aluminium hydroxide, boron nitride, boron nitride, silicon dioxide, titanium oxide microparticle, low order acidify チ Application microgranule, zinc oxide fine particles, the cerium oxide microgranule, active inhibition type cerium oxide microgranule etc.; The example of organic dust has: polyamide powder, polyester powder, polyethylene powders, polypropylene powder, the polystyrene powder, polyurethane powder, the benzoguanamine powder, polymethyl-benzene guanamines powder, polytetrafluorethylepowder powder, the polymethyl methacrylate powder, cellulose, the silk powder, nylon powder, 12 nylon, 6 nylon, silicone powder, silicone rubber powder, the silicone elastomer globular powder, the poly methyl silsesquioxane globular powder, poly-alkyl silsesquioxane powder, styrene acrylic copolymer, the divinylbenzene styrol copolymer, vinylite, urea resin, phenol resin, fluororesin, silicones, acrylic resin, melmac, epoxy resin, polycarbonate resin, the microcrystalline cellulose powder, starch powder, lauroyl resin etc.; The example of surfactant metal salt powder (metallic soap) has: zinc stearate, aluminium stearate, calcium stearate, magnesium stearate, Grillocin P 176, magnesium myristate, cetyl zinc phosphate, cetyl calcium phosphate, cetyl zinc phosphate sodium etc.; The example of pearlescent pigment has: titanium oxide coated mica, titanium oxide coated mica, bismuth oxychloride, titanium oxide coating bismuth oxychloride, titanium oxide coating Talcum, guanin, titanium oxide coat painted Muscovitum etc.With above-mentioned same, can implement various surface treatments to these pigment.
(F) pure water mixes with the scope of 5-25 quality % with respect to solid-state cosmetics total amount.The combined amount of pure water is less than above-mentioned lower limit, and then good sensory deprivation surpasses above-mentioned higher limit, then may damage stability of formulation.Pure water also can use ultra-pure water, mineral water, thermal water etc.
The solid-state shape cosmetics of gained are that outward appearance is a solid, make its mobile dosage form by embrocating, and filling is used in airtight container.The concrete purposes of solid-state cosmetics of the present invention is not particularly limited, and is suitably for beautification product, be particularly suitable for foundation cream, cover up apply some make up, eye shadow cream, lipstick, be suitable as skin nursing product, anti-ultraviolet product, or as daily sun-screening agent.
As mentioned above, we find that M4Q is fit to the various cosmetics that preparation has excellent specific property, but in the manufacture method, as 1,1,1 of by-product generation, 5,5,5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes (below can be described as M3Q (0H)) can cause big problem aspect sensation.That is, 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy group-when 3-hydroxyl trisiloxanes is on the skin with liquid,, show the sliding sense in not preferred intensive surface as cosmetics.After smearing, made skin have harsh feeling within about 5 minutes, passed through about 10 minutes again, volatilization reverts to original skin feel fully, gives sensuously to change greatly.
Carry out various researchs for this reason, found that preferred 1,1,1,5,5, the amount of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes is 1.0 quality % or following in cosmetics, more preferably 0.5 quality % or following, further preferred 0.35 quality % or following.In order to make 1,1,1,5,5, the content of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes preferably is about 3 quality % or following in M4Q in above-mentioned scope as can be known, 1.0 quality % or following more preferably from about, further preferred about 0.5 quality % or following.But, 1,1,1,5,5, the boiling point of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes and M4Q is approaching, and according to the difference of synthetic method, its mixed volume is more than 3 quality %, purifies by distillation and removes, and then needs considerable time, energy and cost.Therefore, to making 1,1,1,5,5, the remaining of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes studied for the preparation method of minimal M4Q.Found that: by containing the method for following step (1)-(4):
(1) mix 2-10 mole hexamethyl disiloxane, 0.01-0.5 equimolar acid catalyst in 1 mole of following tetraalkoxysilane, temperature is set at 0 ℃ or above but less than 30 ℃ step;
(2) step of 1 mole of tetraalkoxysilane of adding in the system of step (1) gained;
(3) keeping temperature is 0 ℃ or above but less than 30 ℃, and interpolation 2.5-10.0 mole of water in the system of gained to step (2) in is simultaneously reacted 30 minutes-5 hours step; And
(4) 30 minutes-5 hours step of reaction under 30-100 ℃ temperature,
Make the hexamethyl disiloxane shown in tetraalkoxysilane shown in the following general formula (A) and the following chemical formula (B)
Si(OR)
4 (A)
(R represents that carbon number is the 1 valency alkyl of 1-10)
(CH
3)
3SiOSi(CH
3)
3 (B)
The material of prepared in reaction, its 1,1,1,5,5, the amount of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes is few, need not can realize above-mentioned about 3 quality % or following by purifications such as distillations, is fit to cosmetics.Among the present invention, the purity of M4Q for example can be used gas chromatographic analysis, carries out quantitatively with 100 fens rates of area, and its concrete grammar is seen embodiment.
In the formula (A), R is the 1 valency alkyl of carbon number 1-10, and its example has ethyl, n-pro-pyl, isopropyl, normal-butyl, isobutyl group, sec-butyl, the tert-butyl group, n-hexyl, octyl group, 2-ethylhexyl, nonyl, decyl, and R can be the same or different mutually.Wherein, preferred especially ethyl or isopropyl.
This tetraalkoxysilane can use purifying by the synthetic material of conventional method, be need not to purify and can be used by tetrachloro silicane and pure synthetic reactant liquor by the desalination acid reaction.Be generally high-purity by the desalination acid reaction by the not purification tetraalkoxysilane that tetrachloro silicane and alcohol obtain,, contain pure and mild a small amount of disiloxane as impurity.If the purity of the tetraalkoxysilane of not purifying that this reaction is used is 50% or above just no problem, preferred 80% or above purity, preferred especially 90% or above purity.
Above-mentioned preparation method is preferably used the hexamethyl disiloxane of 2-10 mole with respect to 1 mole of tetraalkoxysilane, further preferred 2.5-5.0 mole.Hexamethyl disiloxane is less than 2.0 moles, then reaction intermediate alcoxyl matrix (1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy group-3-methoxyl group trisiloxanes ({ (CH
3)
3SiO}
3SiOCH
3, be designated hereinafter simply as M
3Q (OMe)) or 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy group-3-trisiloxane ethoxylate ({ (CH
3)
3SiO}
3SiOCH
2CH
3, be designated hereinafter simply as M3Q (OEt)) etc.) remaining quantity increase, so reaction yield reduces, even surpass 10.0 moles, also has hopeless yield to improve, the problem that jar (Port Star ト) yield (the overall raw material of unit adds up to the yield of quality) reduces.
In the above-mentioned steps (1), preferably adding 0.5-10.0 mole carbon number with respect to 1 mole of above-mentioned tetraalkoxysilane is the 1 valency lower alcohol of 1-6, its object lesson has methanol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol, amylalcohol, hexanol, particular methanol, ethanol, isopropyl alcohol.
The use amount of 1 valency lower alcohol used herein is the 0.5-10 mole with respect to 1.0 moles of tetraalkoxysilanes, preferred especially 1-5 mole.The amount of 1 valency lower alcohol is less than 0.5 mole, and then the dispersibility of the necessary water of hydrolysis is not enough, and the remaining quantity of reaction intermediate increases or the output of high boiling product increases, and yield is low.Surpass 10 moles, the problem that then has jar yield to reduce.
Tetraalkoxysilane uses chemical formula Si (OCH
3)
4During shown tetramethoxy-silicane, preferably use 2.0-10.0 mole hexamethyl disiloxane with respect to 1 mole of tetramethoxy-silicane, 1.0-5.0 mole is selected from 1 valency lower alcohol of methanol, ethanol, isopropyl alcohol, 0.01-0.5 equimolar acid catalyst, 2.5-10.0 mole of water, the step of adding water is 0 ℃ or above but reaction 30 minutes-5 hours under less than 30 ℃ of temperature, and the interpolation of water finishes back reaction 30 minutes-5 hours under 30-100 ℃ of temperature, the method for the condensation reaction that is hydrolyzed.
R in the tetraalkoxysilane is for the silane except that methyl, particularly when being tetraethoxysilane, tetrapropoxysilane, when hydrolysis carries out, by-product ethanol or propanol, the dispersibility of water and alkoxy silane improves, and therefore the advantage that can not use as 1 valency lower alcohol of solvent is arranged.Consider from the jar yield, especially preferably need not the synthetic method of 1 valency lower alcohol.
The example of acid catalyst has: sulphuric acid, hydrochloric acid, methanesulfonic acid, trifluoromethanesulfonic acid etc.Especially preferably use sulphuric acid, trifluoromethanesulfonic acid.The use amount of acid catalyst is preferably used the 0.01-0.5 mole with respect to 1 mole of tetraalkoxysilane, the further preferred 0.02-0.4 mole that uses.The amount of acid catalyst is less than 0.01 mole, and then response speed is slack-off, and the response time is elongated, surpasses 0.5 mole, and then the output of high boiling substance increases, the problem that has yield to descend.
The water that this reaction is used can use with independent water, also can use to be added with the water of carbon number as the 1 valency lower alcohol of 1-6.When adding 1 valency lower alcohol in the water, this alcohol can be methanol, ethanol, normal propyl alcohol, isopropyl alcohol, n-butyl alcohol, isobutanol etc.The total use amount of 1 valency lower alcohol is preferably in described molar ratio range before.
The use amount of the water that uses in this reaction is preferably used the 2.5-10.0 mole with respect to 1 mole of tetraalkoxysilane, further preferred 3.0-8.0 mole.Trialkoxy silane is less than 2.5 moles, and then the residual quantity as the alcoxyl matrix (M3Q (OMe), M3Q (OEt) etc.) of reaction intermediate increases, and yield reduces, even but surpass 10 moles, the also hopeless raising of its yield, the problem that the generation tank yield reduces.
This reaction is preferred to be earlier that the 1 valency lower alcohol of 1-6 mixes remix acid catalyst and tetraalkoxysilane class with hexamethyl disiloxane and as required carbon number.Also hexamethyl disiloxane, alcohol, acid catalyst, tetraalkoxysilane can be mixed simultaneously, but the temperature that preferably made reactant mixture before adding entry is 0 ℃ or above but less than 30 ℃, be preferably 0 ℃ or above but, be preferably 0 ℃ to 15 ℃ especially less than 25 ℃.Be lower than in temperature under the state of above-mentioned lower limit and add water, then response speed is slack-off, thereby the response time is long; And add water above under the state of above-mentioned higher limit in temperature, then the yield of target substance, M4Q reduces, thereby not preferred.
In order further to improve the productive rate of M4Q, can be with hexamethyl disiloxane and the mixing of 1 valency lower alcohol as required, the temperature that makes mixture is 0 ℃ or above but less than 30 ℃.Preferred 0-25 ℃, preferred 0-15 ℃ especially.To wherein adding acid catalyst, said temperature is no more than 30 ℃ therebetween, preferably is no more than 25 ℃, especially preferably is no more than 15 ℃, stirs 10 minutes-1 hour under this temperature.Then, preferred so that the temperature of reactant mixture remain on 0 ℃ or above but less than 30 ℃ speed, preferably with keep 0-25 ℃ speed, especially preferably to keep 0-15 ℃ speed to add tetraalkoxysilane, under this temperature, stirred 10 minutes-1 hour, add water then.
Therefore preferably this reaction is further to add entry to be hydrolyzed, but adds then heat release of entry, cools off on one side so that 0 ℃ of the temperature maintenance of reactant mixture or above but add less than 30 ℃ temperature.When adding water, internal temperature is less than 0 ℃, and then response speed is slack-off, and the response time is long; And be 30 ℃ or more than, then the yield of object reduces.Preferred interpolation especially preferably keeps 0-15 ℃ of ground to add with keeping 0-25 ℃ of temperature.After adding water and finishing, further preferably at 0 ℃ or above but continue to stir 10 minutes-5 hours less than 30 ℃.
After above-mentioned steps, in this reaction, preferably further reaction mixture temperature is heated to 30-100 ℃, preferred 40-80 ℃, continue to stir 30 minutes-5 hours, preferred 1 hour-3 hours.Like this, reduce as the alcoxyl matrix (M3Q (OMe), M3Q (OEt) etc.) of reaction intermediate and the residual quantity of M3Q (OH), the yield of object M4Q improves.
In this method, preferably after reaction, separate water layer, organic layer is neutralized with aqueous alkalis such as sodium bicarbonate water by separatory.Washing organic layer again, is neutral until washing liquid, distills purification, and the reactant liquor after perhaps will washing adds desiccant such as anhydrous sodium sulfate or calcium chloride and dewaters, and distillation is purified then.
Below, in order to carry out reference, in the past synthetic method is described.The synthetic method that is used to obtain M4Q can be with reference to the synthetic method of methyl three (trimethylsiloxy group) silane (M3T).The method of the known present M3T of preparation has following method.
1. in the presence of methanol, make the method (international open WO 2001-15658 number, TOHKEMY 2002-68930 communique) of methyl trichlorosilane and trim,ethylchlorosilane cohydrolysis.
2. in the presence of the perchloric acid catalysis agent, make the method (Dokl.Akad.Nauk SSSR, 227,607-610 (1976)) of methyl trichlorosilane and hexamethyl disiloxane reaction.
3. in the presence of acid-exchange resin, make the method (J.Organomet.Chem., 340,31-36 (1988)) of MTES and hexamethyl disiloxane reaction.
4. in the presence of carboxylic acid and acid catalyst, make the method (Japanese kokai publication hei 11-217389 communique) of methyl trialkoxysilane and hexamethyl disiloxane reaction.
5. in MTMS, hexamethyl disiloxane and methanol, add concentrated sulphuric acid, drip the method (international open WO 2001-15658 communique, TOHKEMY 2002-68930 communique) that water and methanol mixture are reacted then.
1 method needs a large amount of water, and the selectivity of reaction is low, so yield is very low.
2 method need use the perchloric acid that is difficult to obtain as catalyst, is not suitable as industrial preparation method.
In 3 the method,, need to use excessive greatly hexamethyl disiloxane in order to improve response rate.In methyl three (trimethylsiloxy group) silane synthetic, 5-seven methyl-3-trisiloxane ethoxylate ({ (CH are arranged as 1,1,1,3,5,5 of reaction intermediate
3)
3SiO}
2Si (OCH
2CH
3) CH
3, hereinafter to be referred as M2T (OEt)) a large amount of remaining shortcomings.And, when on silicon atom, importing trimethylsiloxy group, be to import 3 trimethylsiloxy groups during synthesizing methyl three (trimethylsiloxy group) silane, but the 3rd reactivity is lower than the 2nd.During synthetic four (trimethylsiloxy group) silane, be to import 4 trimethylsiloxy groups, therefore, the reactive further reduction of the reactivity of suspecting the 4th trimethylsiloxy group the 3rd trimethylsiloxy group in synthetic than methyl three (trimethylsiloxy group) silane.Therefore, when considering similarly synthetic four (trimethylsiloxy group) silane, more increase, be not suitable as the method that obtains highly purified four (trimethylsiloxy group) silane as the residual quantity of the M3Q (OEt) of reaction intermediate.
In 4 the method, the remaining intermediate M2T (OEt) that responds in methyl three (trimethylsiloxy group) silane synthetic, when therefore similarly synthesizing four (trimethylsiloxy group) silane, the residual quantity of suspecting the M3Q (OEt) as reaction intermediate is more, can not satisfy as the method that effectively obtains highly purified four (trimethylsiloxy group) silane.
In 5 the method, with above-mentioned same, remaining the intermediate { (CH that responds in methyl three (trimethylsiloxy group) silane synthetic
3)
3SiO}
2Si (CH
3) OCH
3(hereinafter to be referred as M2T (OMe)) when therefore similarly synthesizing four (trimethylsiloxy group) silane, suspects that the residual quantity of the M3Q (OMe) as reaction intermediate is more, can not satisfy as the method that effectively obtains highly purified four (trimethylsiloxy group) silane.
Shown in the embodiment table 1 and 2, with respect to above-mentioned method in the past, the method according to this invention can obtain M3Q (OH) about 3 quality % of amount or following product before purifying as described later.
Impurity among the M4Q of preparation can be by gas chromatographic analysis, shown in analysis condition is for example following.
The gas phase chromatographic device GC14B of Shimadzu Seisakusho Ltd.
3% grade of column packing trade name SE30, liquid phase
Column internal diameter 5mm, length 3m
80 ℃ of detector TCD, injection temperatures
Under 80 ℃ of the furnace temperature, 1 minute retention time, 300 ℃ of 15 ℃/minute programming rate, final temperatures
When above-mentioned condition was analyzed, M3Q (OMe) 10.5-13.0 minute between detected multiple 6.6 minutes, M4Q 7.5 minutes, high boiling point composition 6.3 minutes, M3Q (OH) 6.2 minutes, M3Q (OEt).
An example of the physical data of the M4Q that finally obtains is as follows.
Outward appearance: water white liquid
Boiling point: 215 ℃ (1 atmospheric pressure), 89.5-90.0 ℃/1.3kPa
Viscosity: (25 ℃); 3.1mm
2/ s
Proportion: (25 ℃); 0.864
Refractive index: (25 ℃); 1.387
Freezing point :-70 ℃ or following
This M4Q preferably is blended in above-mentioned various cosmetics.In the scope of harmless purpose of the present invention; cosmetics of the present invention are except that above-mentioned each composition; can use the employed various compositions of common cosmetics, for example various compositions such as anti-ultraviolet composition, oil preparation, antiseptic, spice, wetting agent, viscosifier, salt, solvent, antioxidant, chelating agen, nertralizer, pH regulator agent, insect repellent, physiologically active ingredient.
The anti-ultraviolet composition can use the material of inorganic system and organic system.The example of the anti-ultraviolet composition of inorganic system for example has metal-oxides such as titanium dioxide, low order acidify チ Application, zinc oxide, cerium oxide, active enclosed type cerium oxide, metal hydroxidess such as hydrated ferric oxide., foil classes such as tabular ferrum oxide, aluminium flake, ceramic-like such as carborundum.Wherein, be preferably selected from mean diameter metal oxide microparticle or metal hydroxides microgranule at least a in the scope of 5-100nm especially.As above-mentioned pigment, also can implement various surface treatments.
The example of organic system anti-ultraviolet composition is p-methoxycinnamic acid 2-Octyl Nitrite (another name: the p-methoxycinnamic acid monooctyl ester) for example; 2-hydroxyl-4-methoxy benzophenone; 2-hydroxyl-4-methoxy benzophenone-5-sulphuric acid; 2; 2 '-dihydroxy-4-methoxy benzophenone; to methoxyl group hydrocinnamic acid diethanolamine salt; para-amino benzoic acid (hereinafter to be referred as PABA); PABA ethyl dihydroxy propyl ester; PABA glyceride; the high ester of salicylic acid; the methyl o-aminobenzoa; 2-ethylhexyl-2-cyano group-3; 3-diphenylacrylate ester; octyldimethyl PABA ester; salicylic acid octyl group ester; 2-phenyl-benzimidazole-5-sulphuric acid; trolamine salicylate; 3-(4-methyl benzal) Camphora; 2; the 4-dihydroxy benaophenonel; 2; 2 '; 4; 4 '-tetrahydroxybenzophenone; 2; 2 '-dihydroxy-4; 4 '-dimethoxy-benzophenone; 2-hydroxyl-4-N-octyloxy benzophenone; 4-isopropyl diphenyl formoxyl methane; the 4-tert-butyl group-4 '-methoxy dibenzoyl methylmethane; octyl triazone; 4-(3; 4-dimethoxy benzene methylene)-2,5-dioxo-1-imidazolidinyl propanoic acid 2-ethyl hexyl ester; its polymeric derivative; and silane derivative etc.
Can also use organic system anti-ultraviolet composition to be enclosed material in the polymer powder.Polymer powder can be hollow can not be yet, average primary particle diameter can be the scope of 0.1-50 μ m, particle size distribution can be that wide distribution also can be narrow distribution.The kind of polymer has acrylic resin, methacrylic resin, styrene resin, polyurethane resin, polyethylene, polypropylene, polyethylene terephthalate, silicone resin, nylon, acrylamide resin etc.In these polymer powders, preferably, especially preferably mix the UVA absorbent 4-tert-butyl group-4 '-methoxy dibenzoyl methylmethane to enclose the powder of organic system anti-ultraviolet composition in the scope of powder quality 0.1-30 quality %.
In the above-mentioned anti-ultraviolet composition; from commonly used, obtain easily and angle that preventing ultraviolet effect is high is considered, be preferably selected from least a of titanium oxide microparticle, zinc oxide fine particles, p-methoxycinnamic acid 2-ethyl hexyl ester, the 4-tert-butyl group-4 '-methoxy dibenzoyl methylmethane, benzophenone series UV absorbent.Especially preferably inorganic system and organic system are used in combination.Also preferably with corresponding UV-A with being used in combination of corresponding UV-B.
The example of the oil preparation commonly used that uses among the present invention has: American Avocado Tree oil, Semen Lini oil, almond oil, she protects many waxes, Fructus Perillae oil, olive oil, cocoa butter, kapok wax, Semen Torreyae oil, Brazil wax, liver oil, candelilla wax, Adeps Bovis seu Bubali, neat's foot oil, neatsfoot stock, hardened tallow, almond oil, spermaceti, fixed oil, Semen Tritici aestivi germ oil, Oleum sesami, rice germ oil, Testa oryzae oil, sugarcane wax, the Flos Camelliae Japonicae caul-fat, the safranine caul-fat, シ ア バ -, Oleum Verniciae fordii, Oleum Cinnamomi, Jojoba wax, shellac wax, turtle oil, soybean oil, tea-seed oil, Camellia oil, Radix Oenotherae erythrosepalae oil, Semen Maydis oil, Adeps Sus domestica, Oleum Brassicae campestris, Japanese tung oil, bran wax, germ oil, house oil, パ-シ Star Network oil, Petiolus Trachycarpi oil, palm kernel oil, Oleum Ricini, hardened castor oil, the Castor Oil Fatty Acid methyl ester, sunflower oil, grapefruit, Fructus Lauri nobilis wax, ホ ホ バ oil, macadimia nut oil, Cera Flava, ermine oil, Oleum Gossypii semen, cotton wax, vegetable wax, the vegetable wax kernel oil, montan wax, cocos nucifera oil, the hydrogenation cocos nucifera oil, three coconut oil fat acid glycerides, Adeps caprae seu ovis, Oleum Arachidis hypogaeae semen, lanoline, liquid lanolin, the reduction lanoline, lanolin alcohol, the hard lanoline, the acetic acid lanoline, the lanolin fatty acid isopropyl ester, lauric acid hexyl ester, POE lanoline alcohol ether, acetic acid POE lanoline alcohol ester, the lanolin fatty acid macrogol ester, POE hydrogenated lanolin alcohol ether, the yolk wet goods; The example of hydrocarbon ils has: ceresine, squalane, Squalene, ceresin, paraffin, paraffin, liquid paraffin, pristane, polyisobutylene, microwax, vaseline etc.; The example of higher fatty acids has: lauric acid, myristic acid, Palmic acid, stearic acid, mountain Yu acid, 9-undecylenic acid, oleic acid, linoleic acid, linolenic acid, arachidonic acid, eicosapentaenoic acid (EPA), docosahexenoic acid (DHA), isostearic acid, 12-hydroxy stearic acid etc.; The example of the oil preparation of higher alcohol system has: lauryl alcohol, myristyl alcohol, palmityl alcohol, stearyl alcohol, behenyl alcohol, hexadecanol, oleyl alcohol, isooctadecanol, hexyl lauryl alcohol, octyl dodecanol, cetostearyl alcohol, 2-decyl tetradecyl alchohol, cholesterol, plant sterol, POE cholesterol ether, single stearyl glyceryl ether (batilol), single oil base glyceryl ether (selachyl alcohol) etc.; The example of ester oil has: adipic acid diisobutyl ester, adipic acid 2-hexyl decyl ester, adipic acid two-2-heptyl undecyl ester, single isostearic acid N-alkyl diol ester, isostearic acid isocetyl ester, three isostearic acid trihydroxymethylpropanyl esters, two-2 ethyl hexanoic acid glycol ester, the 2 ethyl hexanoic acid cetyl ester, three-2 ethyl hexanoic acid trihydroxymethylpropanyl ester, four-2 ethyl hexanoic acid pentaerythritol ester, sad cetyl ester, octyl group dodecyl ガ system ester, oleic acid oil base ester, oleic acid octyl group dodecyl ester, the oleic acid decyl ester, the different nonyl ester of different n-nonanoic acid, two capric acid DOPCP, triethyl citrate, succinic acid 2-ethyl hexyl ester, acetic acid amyl group ester, ethyl acetate, butyl acetate, stearic acid isocetyl ester, butyl stearate, Dermol DIPS, decanedioic acid two 2-ethyl hexyl ester, the lactic acid cetyl ester, lactic acid meat myristyl ester, isopropyl palmitate, Palmic acid 2-ethyl hexyl ester, Palmic acid 2-hexyl decyl ester, Palmic acid 2-heptyl undecyl ester, 12-hydroxy stearic acid cholesterol ester, the fatty acid dipentaerythritol ester, isopropyl myristate, myristic acid octyl group dodecyl ester, myristic acid 2-hexyl decyl ester, myristic acid myristyl ester, the sad hexyl decyl ester of dimethyl, ethyl laurate, lauric acid hexyl ester, N-lauroyl-L-glutamic acid-2-octyl group dodecyl ester, malic acid two iso stearyl esters etc.; The example of glyceride oil has: acetoglyceride base, three isooctyl acid glyceride, three glyceryl isostearates, three different tripalmitins, three (octyl group capric acid) glyceride, glyceryl monostearate, two-2-heptyl hendecanoic acid glyceride, myristin, myristic acid isostearic acid two glyceride etc.
The compatibility excellence of silicone oil such as the alkyl-modified organopolysiloxane beyond the dimethyl organopolysiloxane, amino modified organopolysiloxane, the organopolysiloxane that contains alcohol hydroxyl group, methyl or phenyl, ア モ ジ メ チ コ-Application and M4Q can preferably be used.The siloxanes chain length of these silicone oil is unqualified, as long as can use in the scope of the degree of polymerization about 1-30000.
Can also mix fluorine such as fluorine modified siloxane, PFPE, the fluorocarbon of fluoridizing Colophonium, perfluorodecalin, PFO etc., fluorinated alcohols, perfluoroalkyl alkyl ether is oil preparation, obtains having the preparation of characteristic.Particularly fluorine modified siloxane, perfluoroalkyl biphenyl modified siloxane or PFPE are rich in versatility, thereby preferred.
Wetting agent for example has: sugar alcohols such as sorbitol, maltose, maltol, as the cholesterol of sterol, sitosterol, plant sterol, lanosterol etc., glucose, sucrose, lactose, Raffinose, trehalose, xylitol, glycerol, propylene glycol, dipropylene glycol, 3 third glycol, polypropylene glycol, 1, the 3-butanediol, ethylene glycol, diethylene glycol, 2,2'-ethylenedioxybis(ethanol)., diglycerol, polyglycereol, hyaluronic acid and salt thereof, chondroitin sulfate and salt thereof, pyrrolidone carboxylic acid salt, Glucam E-10, PP 25, ethyl cyclophosphadenosine glycoside etc.
The example of viscosifier has: arabic gum, Tragacanth, the arabinose galactan, locust bean gum (angle bean), more create glue, karaya, カ ラ ギ-Na Application, pectin, the sub-(Fructus cydoniae oblongae of agar Fructus cydoniae oblongae), starch (rice, corn, Rhizoma Solani tuber osi, Semen Tritici aestivi), ア Le ゲ コ ロ イ De, ト ラ Application ト ガ system, department of botany's macromolecules such as locust bean gum, xanthan gum, glucosan, succinoglucan, department of microbiology macromolecules such as プ Le ラ Application, collagen, casein, albumin, animals such as gelatin are macromolecule, carboxymethyl starch, starch such as methyl hydroxypropyl starch are macromolecule, methylcellulose, ethyl cellulose, the methyl hydroxy propyl cellulose, carboxymethyl cellulose, hydroxy methocel, hydroxy propyl cellulose, NC Nitroncellulose, cellulose sodium sulfate, sodium carboxymethyl cellulose, crystalline cellulose, the cellulose-based macromolecule at cellulose end, sodium alginate, alginic acid such as propylene glycol alginate are macromolecule, polyvinyl methyl ether, polyvinylpyrrolidone, ethylene base system macromolecules such as CVP Carbopol ETD2050, polyoxyethylene such as Polyethylene Glycol are macromolecule, poloxalkol is a macromolecule, sodium polyacrylate, polyethyl acrylate, acrylic acid series macromolecules such as polyacrylamide, polymine, cationic polymer, bentonite, Magnesiumaluminumsilicate, ラ Port Na イ ト, terre verte, saponite, Strese Hofmann's hectorite., silicic acid anhydrides etc. are inorganic to be viscosifier etc.Other viscosifier have the oil-soluble gelating agent; for example can use and be selected from aluminium stearate; magnesium stearate; metallic soaps such as Grillocin P 176; N-lauroyl-L-glutamic acid; α; amino acid derivativges such as γ-di-n-butylamine; the dextrin cetylate; the dextrin stearate; dextrin fatty acid esters such as dextrin 2 ethyl hexanoic acid cetylate; sucrose palmitate; sucrose fatty acid ester such as sucrose stearate; single benzylidene sorbitol; the benzylidene derivatives of sorbitol such as dibenzyl sorbitol, dimethyl benzyl dodecyl ammonium montmorillonitic clay; the dimethyl dioctadecyl ammonium DDA N,N-Dimethyl-N-octadecyl-1-octadecanaminium Montmorillonitum; at least a gelating agent of organo-clay mineral such as octadecyl dimethyl benzyl ammonium Montmorillonitum etc.
Surfactant can also suitably use the surfactant of anionic property, cationic according to the kind of preparation except that above-mentioned nonionic.Anionic surfactant's example has: fatty acid soaps such as sodium stearate or Palmic acid triethanolamine, alkyl ether carboxylic acid and salt thereof, the carboxylate of aminoacid and fatty acid condensation etc., alkyl sulfonic acid, sulfonated alkene, the sulfonate of fatty acid ester, the sulfonate of fatty acid amide, the sulfonate of alkylsulfonate and formaldehyde condensation products thereof, alkyl sulfate salt, senior secondary alcohol sulfuric acid, alkyl and allyl ether sulfuric acid, the sulfuric acid of fatty acid ester, the sulfuric acid of fatty acid alkyl alcohol amide, the sulfuric ester salt of Turkey red wet goods, alkylphosphonic, ether phosphate, alkyl allyl ether phosphate, amidophosphoric acid salt, the N-acylamino acid is an activating agent etc.; The example of cationic surfactant has: amine salt such as alkylamine salt, polyamines and amino alcohol fatty acid derivatives, alkyl quaternary ammonium salts, aromatics quaternary ammonium salt, pyridiniujm, imidazole salts etc.
Examples of preservatives has: alkyl paraben, benzoic acid, sodium benzoate, sorbic acid, potassium sorbate, phenyl phenol etc.; The example of antibacterial has: benzoic acid, salicylic acid, carbolic acid, sorbic acid, alkyl paraben, to chloro metacresol, hexachlorophenol, benzyl chloride alkanamine, chlorination hibitane, trichlorine carbanilide, triclosan, sensitization element, phenyl phenol etc.
Physiologically active ingredient can be when being applied in skin, gives the material of some physiologically actives of skin.For example anti-inflammatory agent, age resister, ultraviolet screening agent, tighten up agent, antioxidant, hair growth promoter, educate a mao agent, wetting agent, blood circulation accelerant, antibacterial, biocide, desiccant, freshener, temperature sense agent, vitamins, aminoacid, wound healing promoter, stimulate demulcent, analgesics, cell vitalizing agent, enzyme component etc.Wherein preferred especially natural series plant extract composition, Sargassum are extracted composition, crude drug composition.Among the present invention, preferably mix these physiologically active ingredients more than a kind or 2 kinds.
The example of these physiologically active ingredients has: eight zhang grass (ァ シ バ) extract, American Avocado Tree (ア ボ ガ De) extract, sweet tea (ア マ チ ヤ) extract, Althaea officinalis L. (ァ Le テ ア) extract, Arnica montana (ア Le ニ カ) extract, Aloe (ア ロ エ) extract, Fructus Pruni extract, the Semen Armeniacae Amarum extract, Semen Ginkgo extrac, Fructus Foeniculi extract, Rhizoma Curcumae Longae (ウ コ Application) extract, oolong tea extract, Fructus Rosae (エ イ ジ Star) extract, Echinacea Species (エ チ Na シ) leaf extract, Radix Scutellariae extract, Cortex Phellodendri extract, Rhizoma Coptidis extract, Fructus Hordei Vulgaris extract, Radix Hyperici Monogyni (Herba Hyperici Monogyni) (オ ト ギ リ ソ ウ) extract, Herba lamii barbati (オ De リ コ ソ ウ) extract, Herba Oenanthes Javanicae (オ ラ Application ダ カ ラ シ) extract, the orange extract, the dry thing of sea water, Sargassum extract, the hydrolysis elasticin, the hydrolyzed wheat powder, hydrolyzed-silk, Chamomile (カ モ ミ ラ) extract, Radix Dauci Sativae (カ ロ Star ト) extract, Herba Artemisiae Scopariae (カ ワ ラ ヨ モ ギ) extract, Radix Glycyrrhizae extract, Flos Hibisci Mutabilis (カ Le カ デ) extract, fire sour jujube (カ キ ヨ Network) extract, Fructus actinidiae chinensis (キ ウ イ) extract, quinine (キ Na) extract, Fructus Cucumidis sativi (キ ュ-カ Application バ-) extract, guanosine, Flos Gardeniae (Network チ Na シ) extract, Indocalanmus tessellatus (Network マ ザ サ) extract, Sophora japonica L. (Network ラ ラ) extract, Semen Juglandis (Network Le ミ) extract, grapefruit extract, Network レ マ テ イ ス extract, chlorella (Network ロ レ ラ) extract, the Mulberry extract, Radix Gentianae (ゲ Application チ ア Na) extract, black tea extract, yeast extract, Fructus Arctii (go ボ ウ) extract, the Testa oryzae fermented product extract, rice germ oil, Bellis perennis (コ Application Off リ-) extract, collagen, Pericarpium Citri tangerinae (コ ケ モ モ) extract, Herba Asari (サ イ シ Application) extract, Radix Bupleuri (サ イ コ) extract, umbilical cord (サ イ イ) extracting solution, Salvia japonica Thunb. (サ Le PVC ァ) extract, Saponaria officinalis (サ ボ Application ソ ウ) extract, bamboo (サ サ) extract, Fructus Crataegi (サ Application ザ シ) extract, Pericarpium Zanthoxyli (サ Application シ ヨ ウ) extracting solution, Lentinus Edodes (シ イ ケ) extract, Radix Rehmanniae (ジ オ ウ) extract, Rhizoma Seu Herba Bergeniae (シ コ Application) extract, Folium Perillae (シ ソ) extract, Hibiscus syriacus (シ Na ノ キ) extract, Ramulus et Folium Spiraeae Salicifolia (シ モ Star ケ ソ ウ) extract, Radix Paeoniae (シ ヤ Network ヤ Network) extract, Rhizoma Acori Graminei (シ ヨ ウ Block) root extract, Betula platyphylla Suk. (シ ラ カ バ) extract, Herba Equiseti Hiemalis's (ス ギ Na) extract, the ocean Caulis Hederae Sinensis extract, Europe Fructus Crataegi (セ イ ヨ ウ サ Application ザ シ) extract, Sambucus nigra L. (セ ィ ヨ ウ ニ ワ ト コ) extract, achillea millefolium (セ イ ヨ ウ ノ コ ギ リ ソ ウ) extract, lavender (セ イ ヨ ウ Ha Star カ) extract, Salvia japonica Thunb. (the extract of セ-ジ), Radix Malvae sylvestris (ゼ ニ ア オ イ) extract, Rhizoma Chuanxiong (セ Application キ ユ ウ) extract, Herba Swertiae bimaculatae (セ Application Block リ) extract, Semen sojae atricolor (ダ イ ズ) extract, Fructus Jujubae ( イ ソ ウ) extract, Herba thymi vulgaris ( イ system) extract, tea extract, Flos Caryophylli (チ ヨ ウ ジ) extract, Herba Imperatae (チ ガ ヤ) extract, Pericarpium Citri Reticulatae (チ Application ピ) extract, Radix Angelicae Sinensis (ト ウ キ) extract, ト ウ キ Application セ Application カ extract, Semen Persicae extract, PiceameyeriRehd. Et Wils. (ト ウ ヒ) extract, Herba Houttuyniae (De Network ダ ミ) extract, Fructus Lycopersici esculenti extract, natto extract, Radix Ginseng extract, the Bulbus Allii extract, Flos rosae multiflorae (ノ バ ラ) extract, Hibiscus syriacus L. (Ha イ PVC ス カ ス) extract, Radix Ophiopogonis (バ Network モ Application De ウ) extract, lotus (Ha ス) extract, parsley (パ セ リ) extract, Mel, Radix Hamamelidis Mollis (Ha マ メ リ ス) extract, wall pellitory (パ リ エ リ ア) extract, Japan's Mazus japonicus (ヒ キ オ コ シ) extract, bisabolol, the Folium Eriobotryae extract, coltsfoot (Off キ Application Port Port) extract, Petasites officinalis Moench (Off キ ノ ト ウ) extract, Poria (Block Network リ ヨ ウ) extract, Block Star チ ヤ-Block Le-system extract, Fructus Vitis viniferae extract, propolis, Fructus Luffae (ヘ チ マ) extract, Flos Carthami (ベ ニ バ Na) extract, mentha leave (ペ パ-ミ Application ト) extract, tilia miqueliana (ボ ダ イ ジ ユ) extract, Paeonia suffruticosa (ボ Application) extract, hops (ホ Star プ) extract, pinaster (マ Star) extract, Aesculus chinensis Bunge (マ ロ ニ エ) extract, Microsorium dilatatum (Bedd.) Sledge (ミ ズ バ シ ヨ ウ) extract, Fructus Sapindi Mukouossi (system Network ロ ジ) extract, Herba melissae axillaris (メ リ Star サ) extract, the peach extract, Centaurea cyanus (ヤ グ Le マ ギ Network) extract, Eucalyptus (ユ-カ リ) extract, Herba Saxifragae (ユ キ ノ シ ) extract, Fructus Citri grandis (ユ ズ) extract, Semen Coicis (ヨ Network イ ニ Application) extract, Radix Artemisia ordosicae (ヨ モ ギ) extract, lavandula angustifolia (ラ ベ Application ダ-) extract, Fructus Mali pumilae extract, Caulis et Folium Lactucae sativae (レ ス) extract, citron extract, Herba Astragali Melilotoidis (Herba Astragali Sinici) (レ Application ゲ ソ ウ) extract, rose extract, Herba Rosmarini Officinalis (ロ-ズ マ リ-) extract, the Anthemis nobilis extract, Lac regis apis (ロ-ヤ Le ゼ リ-) extract etc.
Also has DNA (deoxyribonucleic acid), mucopolysaccharide, hyaluronate sodium, sodium chondroitin sulfate, collagen, elasticin, chitin, chitosan, biopolymer such as hydrolysed egg shell membrane, glycine, valine, leucine, isoleucine, serine, threonine, phenylalanine, arginine, lysine, aspartic acid, glutamic acid, cystine, cysteine, methionine, aminoacid such as tryptophan, estradiol, hormones such as ethenyl estradiol, aminoacid, sodium lactate, carbamide, pyrrolidone sodium carboxylate, betanin, the composition of preserving moisture such as milk surum, sheath ammonia ester, ceramide, cholesterol, cholesterin derivative, oiliness compositions such as phospholipid; Anti-inflammatory agents such as episilon amino caproic acid, glycyrrhizic acid, β-glycyrrhetin hydrochlorate, lysozyme chloride, Kessazulen, hydrocortisone, allantoin, tranamic acid, azulene; Vitamin A, B2, B6, C, D, E, calcium pantothenate, biotin, nicotiamide, vitaminss such as vitamin C ester, allantoin, dicloavit, 4-amino methyl cyclohexane-carboxylic acid isoreactivity composition, tocopherol, carotenoid, flavonoid, tannic acid, xylan, saponin, Butylated hydroxyanisole, dibenzylatiooluene, antioxidants such as phytic acid, 'alpha '-hydroxy acids, cell vitalizing agent such as beta-hydroxy acid, gamma oryzanol, blood circulation accelerants such as vitamin e derivative, retinol, wound curing agents such as retinol derivatives, cepharanthine, Radix Glycyrrhizae extract, capsicum tincture, Hinokitiol, iodate Bulbus Allii extract, Pyridoxine Hydrochloride, the d1-alpha-tocopherol, acetic acid d1-alpha-tocopherol, nicotinic acid, nicotinic acid derivates, calcium pantothenate, D-panthenol, acetyl pantoyl benzyl ethyl ether, biotin, allantoin, isopropyl methyl phenol, estradiol, ethinylestradiol, chlorination カ プ ロ ニ ウ system, the benzyl chloride alkanamine, diphhydramine hydrochloride, カ Na-Le, Camphora, salicylic acid, n-nonanoic acid vanilla amide, nonane acid vanilla amide, ピ ロ Network ト Application オ ラ ミ Application, pentadecanoic acid glyceride, the 1-menthol, fresheners such as Camphora; Hair growth promoters such as one nitroguaiacol, resorcinol, γ-An Jidingsuan, GABOB, benzethonium chloride, hydrochloric acid mexiletine, auxin, estrogen, Mylabris tincture, cyclosporine, pyrrole sulfur zinc, hydrocortisone, Minoxidil, monostearate polyoxyethylene sorbitan, Oleum menthae, サ サ ニ シ キ extract etc.
The example that PH adjusts agent has lactic acid, citric acid, glycolic, succinic acid, tartaric acid, d1-malic acid, potassium carbonate, sodium bicarbonate, ammonium bicarbonate etc., and the example of chelating agen has: alanine, edetic acid sodium salt, polyphosphate sodium, Polymeric sodium metaphosphate., phosphoric acid etc.
The example of solvent has: in addition water such as pure water, mineral water, deep seawater also have light liquid isoparaffin, ethers, LPG, N-Methyl pyrrolidone, inferior generation プ ロ Application etc.
Except that above-mentioned, the cosmetics that contain M4Q can be skin-protection product, hair preparation, antiperspirant goods, beautification product, anti-ultraviolet goods, aroma material preparation etc.Emulsion, cream, dew, calamine lotion, sunscreen, cosmetic backing material, suntan are for example arranged, shave back skin care liquid, the preceding washing liquid that shaves, face film agent, cleaning agent, the agent of washing one's face, at acne apply some make up, basic cosmetics such as essence, cosmetics such as foundation cream, white lead, eye shadow cream, eyeliner, brow, チ-Network, nail polish paste, lip pomade, lipstick, refreshingly flood, setting agent, talcum powder, educate a mao agent, deodorizer, depilatory, soap, bath essence, balneation agent, hand soaps, perfume etc. at shampoo, Rinsing, conditioner, hair dye.Form for goods is not particularly limited, and can be aqueous, emulsion form, creamy, solid, shaped, paste, gel, Powdered, multilamellar shape, mousse shape, spray shape etc.
Embodiment
Below use embodiment, comparative example to describe the present invention in detail, but the present invention is not limited by these.If no special instructions, the unit of following combined amount adopts quality %.
Preparation embodiment (preparation of four (trimethylsiloxy group) silane))
According to the adding proportion of table 1, table 2,, obtain four (trimethylsiloxy group) silane according to the following step 1-6 reaction that is hydrolyzed.
By following step preparation four (trimethylsiloxy group) silane.
(step 1) is installed reflux condensing tube, thermometer and blender on the four-hole glass flask of 1000ml, replace with nitrogen inside.Add hexamethyl disiloxane and alcohol in this flask, cool off in ice-water bath, making internal temperature is 10 ℃.
(step 2) keeps internal temperature is 10 ℃, wherein drips acid catalyst with 30 fens clockwise, directly stirs 30 minutes under 10 ℃ of temperature.
(step 3) is followed, and keeping internal temperature is 10 ℃, wherein drips alkoxy silane with 45 fens clockwise, directly stirs 1 hour under this temperature.
(it is 10 ℃ that step 4) keeps internal temperature, with 1 hour dropping water, after dropping finishes, stirs 1 hour down at 5-25 ℃ again.
(the step 5) heating, making internal temperature is 50 ℃, stirs 2 hours.
(step 6) is gained reactant liquor separatory, separates water layer, then with organic layer with sodium bicarbonate water, wash with water then.(the gained organic layer is carried out the result of gas chromatographic analysis shown in table 1, table 2.)
[analytical conditions for gas chromatography]
Operative installations: island Tianjin system GC14B
Column packing: trade name SE 30 (3% grade of liquid phase, column internal diameter 5mm, length 3m)
Detector: TCD
The post injection temperature: 80 ℃, the retention time under 80 ℃ is 1 minute, 15 ℃/minute of programming rates, 300 ℃ of final temperatures
Distillation gained organic layer takes out 89.5-90.0 ℃/1.3kPa of boiling point fraction, obtains purity 99.5% or above four (trimethylsiloxy group) silane.
[distillation condition]
Distilling apparatus uses McMahon packing, uses the distillation column of internal diameter 2.5cm, length 70cm.The evaluation of impurity and target substance is analyzed by mass spectrum and NMR and is carried out.
Table 1
| Substance | Preparation embodiment 1 | Preparation embodiment 2 | Preparation embodiment 3 | Preparation embodiment 4 |
Step 1 | Hexamethyl disiloxane | (486.0g 3.0 moles) | (648.0g 4.0 moles) | (486.0g 3.0 moles) | (486.0g 3.0 moles) |
Alcohol | Methanol 96.0g (3.0 moles) | Methanol 96.0g (3.0 moles) | Do not have | Ethanol 46.0g (1.0 moles) |
Step 2 | Acid catalyst | Concentrated sulphuric acid 9.8g (0.1 mole) | Concentrated sulphuric acid 9.8g (0.1 mole) | Concentrated sulphuric acid 9.8g (0.1 mole) | Trifluoromethanesulfonic acid 7.5g (0.05 mole) |
Step 3 | Tetramethoxy-silicane | (152.0g 1.0 moles) | (152.0g 1.0 moles) | - | - |
Tetraethoxysilane | - | - | (208.0g 1.0 moles) | (208.0g 1.0 moles) |
Step 4 | Water | (90.0g 5.0 moles) | (90.0g 5.0 moles) | (90.0g 5.0 moles) | (72.0g 4.0 moles) |
Analysis result | | | | | |
Organic layer analysis midway (GC analysis result) (area %) | M3Q(OMe) | 5.2 | 1.8 | - | - |
M3Q(OEt) | - | - | 4.5 | 6.7 |
M3Q(OH) | 1.1 | 0.3 | 0.9 | 1.8 |
Four (trimethylsiloxy group) silane | 91.7 | 97.2 | 93.4 | 89.6 |
High boiling substance | 2.0 | 0.7 | 1.2 | 1.9 |
The distillation result | Receipts amount (g) | 332.2 | 361.0 | 344.1 | 316.0 |
Yield (%) | 86.5 | 94.0 | 89.6 | 82.3 |
Jar yield (%) | 39.8 | 36.3 | 41.0 | 40.9 |
The GC analysis result (area %) of final purification thing | M3Q(OMe) | Less than 0.1 | Less than 0.1 | - | - |
M3Q(OEt) | - | - | Less than 0.1 | Less than 0.1 |
M3Q(OH) | Less than 0.1 | 0.3 | 0.2 | Less than 0.1 |
Four (trimethylsiloxy group) silane | 99.9 or more than | 99.7 | 99.8 | 99.9 or more than |
High boiling substance | Less than 0.1 | Less than 0.1 | Less than 0.1 | Less than 0.1 |
Table 2
| Substance | Preparation embodiment 5 | Preparation embodiment 6 |
Step 1 | Hexamethyl disiloxane | (405.0g 2.5 moles) | (486.0g 3.0 moles) |
Alcohol | Methanol 96.0g (3.0 moles) | Ethanol 46.0g (1.0 moles) |
Step 2 | Acid catalyst | Concentrated sulphuric acid 19.6g (0.2 mole) | Concentrated sulphuric acid 9.8g (0.1 mole) |
Step 3 | Tetramethoxy-silicane | (152.0g 1.0 moles) | - |
Tetraethoxysilane | - | (152.0g 1.0 moles) |
Step 4 | Water | (90.0g 5.0 moles) | (144.0g 8.0 moles) |
Analysis result | | | |
Organic layer analysis midway (GC analysis result) (area %) | M3Q(OMe) | 8.7 | - |
M3Q(OEt) | - | 4.4 |
M3Q(OH) | 3.1 | 0.6 |
Four (trimethylsiloxy group) silane | 84.2 | 94.1 |
High boiling substance | 4.0 | 0.9 |
The distillation result | Receipts amount (g) | 309.1 | 346.4 |
Yield (%) | 80.5 | 90.2 |
Jar yield (%) | 40.5 | 41.3 |
The GC analysis result (area %) of final purification thing | M3Q(OMe) | Less than 0.1 | - |
M3Q(OEt) | - | Less than 0.1 |
M3Q(OH) | Less than 0.1 | 0.2 |
Four (trimethylsiloxy group) silane | 99.9 or more than | 99.8 |
High boiling substance | Less than 0.1 | Less than 0.1 |
In the table, M3Q (OMe) is { (CH
3)
3SiO}
3SiOCH
3, M3Q (OEt) is { (CH
3)
3SiO}
3SiOCH
2CH
3, M3Q (OH) is { (CH
3)
3SiO}
3SiOH, promptly 1,1,1,5,5,5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes.Yield is obtained by the mol ratio of the tetraalkoxysilane that uses in object four (trimethylsiloxy group) silane and the reaction.
The preparation comparative example
According to the adding proportion shown in the table 3, according to the above-mentioned steps 1-6 reaction that is hydrolyzed, change distillation condition, reclaim the more fraction that contains M3Q (OH), and finely tune with purification four (trimethylsiloxy group) silane, obtain containing the solution of 35%M3Q (OH), 65% 4 (trimethylsiloxy group) silane.The GC analysis result of this solution is as shown in table 4.
Table 3
| Substance | The preparation comparative example |
Step 1 | Hexamethyl disiloxane | (486.0g 3.0 moles) |
Alcohol | Ethanol 46.0g (1.0 moles) |
Step 2 | Acid catalyst | Concentrated sulphuric acid 9.8g (0.1 mole) |
Step 3 | Tetramethoxy-silicane | - |
Tetraethoxysilane | (152.0g 1.0 moles) |
Step 4 | Water | (36.0g 2.0 moles) |
Analysis result | | |
Organic layer analysis midway (GC analysis result) (area %) | M3Q(OMe) | - |
M3Q(OEt) | 0.7 |
M3Q(OH) | 18.2 |
M4Q | 65.8 |
High boiling substance | 15.3 |
Table 4
GC analysis result (area %) | M3Q(OMe) | - |
M3Q(OEt) | |
M3Q(OH) | 35 |
M4Q | 65 |
High boiling substance | 0.1 |
The embodiment and the comparative example of cosmetics of the present invention have below been provided.Below employed four (trimethylsiloxy group) silane (M4Q) be the preparation embodiment 1 in the preparation chemical compound.The TMF-1.5 that methyl three (trimethylsiloxy group) silane (M3T) has adopted chemical industry society of SHIN-ETSU HANTOTAI to make.
Embodiment 1 (cleansing gel)
Prepare cleansing gel according to following prescription and preparation method.
Prescription
(1) ethanol 3.0
(2) glycerol 5.0
(3) dimethyl polysiloxane (annotating 1) 8.0
(4) four (trimethylsiloxy group) silane 15.0
(5) polyether-modified polysiloxanes (annotating 2) 7.0
(6) P.O.E (60 moles) castor oil hydrogenated 1.0
(7) myristic acid octyl group dodecyl ester 2.0
(8) vitamin E (acetate) 0.1
(9) oleyl alcohol 0.3
(10) the alkyl-modified carboxyl group polyvinyl 0.5
(11) CVP Carbopol ETD2050 0.2
(12) methyl parahydroxybenzoate 0.3
(13) potassium hydroxide sends out 0.4
(14) phenyl phenol 0.2
(15) pure water to 100
Annotate 1: シ リ Application KF-96-100cs (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI)
Annotate 2: シ リ コ Application KF-351 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI)
Preparation method:
Oil component uniform mixing dissolving with (1)-(9).Then (10)-(15) uniform mixing is disperseed the oil component of mixed dissolution before adding.Mix dispersion with homogenizer, charge into then in the pipe, obtain goods.
Embodiment 2 (cleansing gel)
According to following prescription, prepare cleansing gel similarly to Example 1.
Prescription
(1) ethanol 3.0
(2) glycerol 5.0
(3) dimethyl polysiloxane (annotating 1) 5.0
(4) four (trimethylsiloxy group) silane 10.0
(5) methyl three (trimethylsiloxy group) silane (M3T) 8.0
(6) polyether-modified polysiloxanes (annotating 2) 7.0
(7) P.O.E (60 moles) castor oil hydrogenated 1.0
(8) myristic acid octyl group dodecyl ester 2.0
(9) vitamin E (acetate) 0.1
(10) oleyl alcohol 0.3
(11) the alkyl-modified carboxyl group polyvinyl 0.5
(12) CVP Carbopol ETD2050 0.2
(13) methyl parahydroxybenzoate 0.3
(14) potassium hydroxide 0.4
(15) phenyl phenol 0.2
(16) pure water to 100
Annotate 1: シ リ コ Application KF-96-100cs (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI)
Annotate 2: シ リ コ Application KF-351 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI)
Comparative example 1
Use volatile cyclic 5 aggressiveness siloxanes to replace four (trimethylsiloxy group) silane, other repeats embodiment 1 fully.
Comparative example 2
Use シ リ コ Application KF-96-100cs (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI) to replace polyether-modified polysiloxanes, P.O.E (60 moles) castor oil hydrogenated, other repeats embodiment 1 fully.
According to following metewand the organoleptic attribute evaluation is carried out in above-mentioned each cleaning agent.
[organoleptic attribute metewand]
Respectively ask 20 professional evaluation personnel (project difference, evaluation personnel repeat sometimes) for each assessment item, in each assessment item, according to being judged as excellent evaluation personnel number, show that by following classification estimates.Following evaluation criterion is all used in later sensory evaluation.
20 philtrums are answered the number for " good " | Estimate |
15 people or above 10-14 people 5-9 people 0-4 people | ◎ ○ △ × |
Evaluation result is as shown in the table.
(organoleptic attribute)
| Use and felt dry sensation afterwards | Makeup removing easily | The usability excellence |
Embodiment 1 embodiment 2 comparative examples 1 comparative example 2 | ◎ ◎ △ ◎ | ◎ ◎ ◎ × | ◎ ◎ ◎ × |
The result of last table shows: embodiments of the invention are compared with comparative example, makeup removing easily, and can not feel dry sensation, the usability excellence.
Embodiment 3 (dried shampoo)
Prepare dried shampoo according to following prescription and preparation method.
Prescription (dried shampoo)
(1) four (trimethylsiloxy group) silane 47
(2) methyl three (trimethylsiloxy group) silane surplus
(3) ethanol 12
(4) methyl phenyl silicone 8
(chemical industry society of SHIN-ETSU HANTOTAI makes KF56)
(5) the different nonyl ester 2 of different n-nonanoic acid
(6) menthol 0.1
(7) spice is an amount of
(8) the Hibiscus syriacus L. extract 0.2
(9) Aloe extract 0.1
Preparation method:
With each composition uniform dissolution, be filled in the container.
Comparative example 3
Use 5 aggressiveness annular siloxanes to replace four (trimethylsiloxy group) silane and methyl three (trimethylsiloxy group) silane of embodiment 3, other prepares fully similarly to Example 3.
Embodiment 4 (scraps of paper shape abluent)
According to following prescription and preparation method, obtain scraps of paper shape abluent.
Prescription (scraps of paper shape abluent)
(1) four (trimethylsiloxy group) silane surplus
(2) ethanol 20
(3) methyl phenyl silicone 4
(chemical industry society of SHIN-ETSU HANTOTAI makes KF56)
(4) 1,3 butylene glycol 10
(5) menthol 0.1
(6) spice is an amount of
Preparation method:
With each composition uniform dissolution, with dispenser solution is injected non-weaving cloth then, with the bag package encapsulation.
Embodiment 5 (scraps of paper shape abluent)
According to following prescription similarly to Example 4, obtain scraps of paper shape abluent.
Prescription (scraps of paper shape abluent)
(1) four (trimethylsiloxy group) silane surplus
(2) methyl three (trimethylsiloxy group) silane (M3T) 25
(3) ethanol 15
(4) methyl phenyl silicone 4
(chemical industry society of SHIN-ETSU HANTOTAI makes KF56)
(5) 1,3 butylene glycol 10
(6) menthol 0.1
(7) spice is an amount of
Comparative example 4
Use the cyclic tetramer volatile siloxane to replace four (trimethylsiloxy group) silane of embodiment 4, other prepares fully similarly to Example 4.
According to above-mentioned functional properties evaluation classification, estimate each abluent, the result is as shown in the table.
(organoleptic attribute)
| Do not feel dry sensation after the use | Easy decontamination dirt | The usability excellence |
Embodiment 3 comparative examples 3 embodiment 4 embodiment 5 comparative examples 4 | ◎ × ◎ ◎ × | ○ △ ◎ ◎ △ | ○ △ ◎ ◎ △ |
The result of last table shows that embodiments of the invention are compared with comparative example, decontamination easily, and can not feel dry sensation, the usability excellence.
The prescription of the spice that uses among the embodiment 3-5 is as shown in the table.
Fragrance formulations |
Composition | Quality ‰ | Composition | Quality ‰ |
Terpinol | 10.00 | Vanillin | 2.00 |
Tirpinyl acetate | 2.00 | Vanillal | 0.10 |
セピオネ-ト | 60.00 | Muscone | 0.50 |
MDJ | 250.00 | The tridecandioic acid ethyl | 42.00 |
Indole | 0.05 | 4,6,6,7,8,8-hexamethyl-1,3,4,6,7,8-six hydrogen ring pentaphene and pyrans | 60.00 |
2-methyl-3-(3,4-methylene dioxy-phenyl)-propionic aldehyde | 3.00 | Pentadacanolide | 20.00 |
Hydroxycitronellal | 20.00 | Ambrettolide (ァ Application Block レ Star ト ラ イ De) | 1.00 |
Hydroxycitronellol | 10.00 | Peach aldehyde | 0.40 |
Right-tert-butyl group-the Alpha-Methyl hydrocinnamaldehyde | 35.00 | Decanolactone | 0.10 |
4-(4-hydroxy-4-methyl-amyl group)-3-cyclohexene-1-カ Le ボ キ シ ア Le デ ヒ De | 75.00 | 4-(4-hydroxy phenyl)-2-butanone | 0.50 |
3-methyl-5-phenyl amylalcohol | 20.00 | Muscone | 0.10 |
Phenylethanol | 10.00 | Scatol | 0.01 |
α-Zi Luolantong | 10.00 | Cis-jasmone | 0.05 |
Alpha, beta-lonone | 20.00 | Ethyl phenyl acetate | 0.10 |
Cetone gamma | 10.00 | Civetone | 0.20 |
Dihydro- | 25.00 | γ-n-nonanoic acid lactone | 0.05 |
Benzyl salicylate | 150.00 | α-santalol | 0.20 |
Cis-3-hexenyl salicylate | 30.00 | β-santalol | 0.20 |
Acetaminol | 0.80 | Acetic acid clove tree ester | 0.10 |
Cinnamyl alcohol | 5.00 | Jasmonal H | 20.00 |
Cinnamic aldehyde | 0.50 | α-damascone | 0.04 |
The acid guaiacyl alcohol ester | 1.00 | β-damascone | 0.02 |
3,8-dimethyl-5-(.alpha.-hydroxyisopropyl)-.DELTA.9-octahydroazulene | 0.50 | Beta-damascenone | 0.01 |
Cedryl acetate. | 5.00 | δ-damascone | 0.01 |
Cupressus funebris Endl. ylmethyl ketone | 30.00 | Rose absolute | 0.50 |
6,7-dihydro-1,1,2,3,3-pentamethyl-4 (5H)-indane | 2.00 | Oleum Rosae Rugosae | 4.50 |
Vetacetyl | 10.00 | Sandalwood oil | 2.00 |
3-methyl-5-(2,3,3-trimethyl-3-cyclopentenes-1-yl)-pentane-2-alcohol | 2.00 | Labdanum absolute | 0.05 |
2-ethyl-4-(2,3,3-trimethyl-3-cyclopentenes-1-yl)-2-butylene-1-alcohol | 0.80 | シ ス ト absolute oil | 0.01 |
The isobornyl Hexalin | 35.00 | Vetiver oil | 0.50 |
Piperonal | 10.00 | Guaiac wood oil | 0.10 |
Coumarin | 2.00 | Add up to | 1000.00 |
Embodiment 6 (lipstick)
Prepare lipstick according to following prescription and preparation method.Coloring pigment uses with 8 quality %N
εThe pigment that-lauroyl-L-lysine is handled, mica titanium is used the pigment of handling with the same substance of 10 quality %.Titanium oxide uses with 8 quality % octyl group silane treatment.
(preparation of coloring pigment dispersion liquid)
In red No. 201 of 30 mass parts surface treatments, mix 70 mass parts four (trimethylsiloxy group) silane.Then, make dispersion liquid A with sand mill mill twice.
In red No. 202 of 30 mass parts surface treatments, mix 70 mass parts four (trimethylsiloxy group) silane.Then, make dispersion liquid B with sand mill mill twice.
Prescription
(composition A)
(1) dispersion liquid A 3
(2) dispersion liquid B 8
(3) four (trimethylsiloxy group) silane 30
(composition B)
(4) ceresin 18
(5) Oleum Ricini surplus
(6) polybutene 8
(7) alkyl-modified siloxanes 1
(composition C)
(8) handle titanium oxide 1
(components D)
(8) handle mica titanium 14
Preparation method
With composition B mixed dissolution, blending constituent A to wherein dispersion component C and kneading, adds components D at last then, and homodisperse with its degassing, is poured in the mould then, and cooling curing obtains goods.
Comparative example 5
Use ring-type pentamer siloxanes (decamethylcyclopentaandoxane) to replace four (trimethylsiloxy group) silane, other repeats embodiment 6 fully.
Comparative example 6
Dispersion liquid A and the dispersion liquid B that uses among the embodiment 8 do not pulverized with sand mill, only stir, use this solution, preparation method is changed into following, in addition repeat embodiment 6 fully.
Preparation method
With composition B mixed dissolution, mix then and dispersion component C, mediate, add composition A, components D and dispersion then.With its degassing, to pour into then in the mould, cooling curing obtains goods.
Following table is represented the organoleptic attribute evaluation result of the embodiment of the invention 6 and comparative example 5,6.
(organoleptic attribute)
| Bright-colored | Transparent feel is arranged | It is level and smooth to smear sense | Be difficult to fade |
Embodiment 6 comparative examples 5 comparative examples 6 | ◎ △ × | ◎ △ × | ◎ ○ × | ○ ○ × |
Comparison shows that of last table embodiment and comparative example: embodiments of the invention are bright-colored, have transparent feel, smear sense smoothly, are difficult to fade.And comparative example 5 is to use the example that in the past is used as the annular siloxane of dispersant, even degree of scatter is low under same preparation condition, tone goods is variant.Comparative example 6 is not carry out dispersive example, is the quality when in the past using as lipstick.
Embodiment 7 (lipstick)
Prepare lipstick according to following prescription and preparation method.
Pigment uses with 5 quality %N
εThe pigment that-lauroyl-L-lysine is handled.
Prescription
(composition A)
(1) four (trimethylsiloxy group) silane 40
(2) trimethylsiloxy group silicic acid 2
(composition B)
(3) ceresin 18
(4) Oleum Ricini surplus
(5) polybutene 8
(composition C)
(6) handle red No. 202 1
(7) handle titanium oxide 1
(8) handle mica titanium 15
Preparation method
With composition B mixed dissolution, disperse then and mixing composition C, add prior dissolved composition A again, homodisperse with its degassing, is poured in the mould then, and cooling curing obtains lipstick.
Embodiment 8
According to following prescription, prepare lipstick similarly to Example 7.
(1) four (trimethylsiloxy group) silane 20
(2) methyl three (trimethylsiloxy group) silane (M3T) 20
(3) trimethylsiloxy group silicic acid 3
(4) ceresin 8
(5) Oleum Ricini 17
(6) polybutene 10
(7) methyl phenyl silicone 5
(FZ-209: Japanese ユ ニ カ-company makes)
(8) red No. 202 1
(9) titanium oxide 1
(10) mica titanium 15
Comparative example 7
Use ring-type pentamer volatile siloxane (decamethylcyclopentaandoxane) to replace four (trimethylsiloxy group) silane, other repeats embodiment 7 fully.
Comparative example 8
Use ceresin to replace polybutene, other repeats embodiment 7 fully.
Comparative example 9
Use dimethyl polysiloxane (chemical industry society of SHIN-ETSU HANTOTAI makes KF96A, 100cs) to replace four (trimethylsiloxy group) silane, other repeats embodiment 7 fully.
The organoleptic attribute evaluation result of embodiment 7,8 and comparative example 7-9 is as shown in the table.
(organoleptic attribute)
| Prevent through time shift color excellence | Glossy | Bright-colored | There is not dry sensation | It is level and smooth to smear sense | Spreadability is good |
Embodiment 7 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
Embodiment 8 | ◎ | ◎ | ◎ | ◎ | ◎ | ◎ |
Comparative example 7 | ○ | △ | △ | × | ○ | ○ |
Comparative example 8 | × | × | × | × | × | × |
Comparative example 9 | × | ○ | △ | △ | × | △ |
The result of last table shows: embodiments of the invention are compared with comparative example, and projects all have excellent performance.Comparative example 7 is to use the annular siloxane that in the past used to replace the example of four (trimethylsiloxy group) silane, and discovery can be experienced dry sensation, and brightly painted degree is also variant.Comparative example 8 is to use ceresin to replace the situation of polybutene, and it is poor to estimate.Comparative example 9 is not use volatile material and the situation of using the fixedness siloxanes, estimates whole variation.
Embodiment 9
Obtain the solid, shaped foundation cream according to following prescription and preparation method.Pigment uses with 5 quality %N
εThe pigment that-lauroyl-L-lysine is handled.
Prescription
[pigment component] (38.2 quality %)
(1) handles spherical titanium oxide (average primary particle diameter 0.4 μ m) 18
(2) handle ferrum oxide (mixture of iron oxide black, iron oxide red, iron oxide yellow) 1.7
(3) handle Talcum 6
(4) handle Muscovitum 2
(5) N
ε-lauroyl-L-lysine 3.5
(6) poly-alkyl methyl silsesquioxane 5
(average primary particle diameter 4 μ m)
(7) octyl group silylanizing titanium oxide microparticle 2
(average primary particle diameter 10nm)
[liquid composition]
Volatile siloxane (25 quality %)
(8) four (trimethylsiloxy group) silane 25
Polyhydric alcohol (6.5 quality %)
(9) 1,3 butylene glycol 5
(10) maltol 1
(11) Raffinose 0.5
Surfactant (2 quality %)
(12) the isostearic acid sorbitan ester 2
The oil preparation (5 quality %) of solid-state or paste
(13) paraffin 5
Pure water (12.7 quality %)
(14) pure water 12.7
Oil preparation
(15) dimethyl polysiloxane (6 cs) 3
(16) methyl phenyl silicone 2
(17) the p-methoxycinnamic acid monooctyl ester 2
(18) two sad propylene glycol esters 2
(19) the hexahydroxystearic acid dipentaerythritol ester 0.5
Physiologically active ingredient
(20) raspberry (Network ラ Application ベ リ-) extract 1
Antiseptic
(21) p-Hydroxybenzoate 0.1
Preparation method
The oil-based liquid component is dissolved at 80 ℃ of uniform mixing.To wherein adding the pigment component that is pre-mixed, pulverizes, at 80 ℃ of homodisperse.To wherein adding, carry out emulsifying and disperse in advance in 80 ℃ of uniform mixing, dissolved waterborne liquid component.Then, be filled in the metalware, be positioned in the seal container, obtain the solid, shaped foundation cream the emulsion degassing that obtains.
Embodiment 10
According to following prescription, obtain the foundation cream of solid, shaped similarly to Example 9.
Prescription
[pigment component] (38.2 quality %)
(1) handles spherical titanium oxide (average primary particle diameter 0.4 μ m) 18
(2) handle ferrum oxide (mixture of iron oxide black, iron oxide red, iron oxide yellow) 1.7
(3) handle Talcum 6
(4) handle Muscovitum 2
(5) N
ε-lauroyl-L-lysine 3.5
(6) poly-alkyl methyl silsesquioxane 5
(average primary particle diameter 4 μ m)
(7) octyl group silylanizing titanium oxide microparticle 2
(average primary particle diameter 10nm)
[liquid composition]
Volatile siloxane (25 quality %)
(8) four (trimethylsiloxy group) silane 15
(9) methyl three (trimethylsiloxy group) silane 10
Polyhydric alcohol (6.5 quality %)
(10) 1,3 butylene glycol 5
(11) maltol 1
(12) Raffinose 0.5
Surfactant (2 quality %)
(13) the isostearic acid sorbitan ester 2
The oil preparation (5 quality %) of solid-state or paste
(14) paraffin 5
Pure water (12.7 quality %)
(15) pure water 12.7
Oil preparation
(16) dimethyl polysiloxane (6cs) 3
(17) methyl phenyl silicone 2
(18) the p-methoxycinnamic acid monooctyl ester 2
(19) two sad propylene glycol esters 2
(20) two seasons penta 4 of hexahydroxystearic acid ester 0.5
Physiologically active ingredient
(21) the raspberry extract 1
Antiseptic
(22) p-Hydroxybenzoate 0.1
Comparative example 10
Use volatile cyclic pentamer siloxanes to replace four (trimethylsiloxy group) silane, other repeats embodiment 9 fully.
Comparative example 11
Use four (trimethylsiloxy group) silane to replace pure water, other repeats embodiment 9 (mixing four (trimethylsiloxy group) silane, 37.7 quality %) fully.
Comparative example 12
Use fixedness dimethyl polysiloxane (10cs) to replace four (trimethylsiloxy group) silane of embodiment 9, other repeats embodiment 9 fully.
Comparative example 13
Use liquid paraffin to replace the polyhydric alcohol of embodiment 9, other repeats embodiment 9 fully.
Comparative example 14
Use liquid paraffin to replace the paraffin of embodiment 9, other repeats embodiment 9 fully.
Comparative example 15
The amount of the paraffin of embodiment 9 is increased to 10 quality %, reduce amount of purified water simultaneously, in addition repeat embodiment 9 fully.
Comparative example 16
The amount of the isostearic acid sorbitan ester of embodiment 9 is kept to 1 quality %, increases amount of purified water simultaneously, in addition repeat embodiment 9 fully.
Comparative example 17
The amount of the isostearic acid sorbitan ester of embodiment 9 is increased to 5 quality %, increase amount of purified water simultaneously, in addition repeat embodiment 9 fully.
Comparative example 18
The amount that makes pure water among the embodiment 9 is 0 quality %, increases the amount of 1,3 butylene glycol simultaneously, in addition repeats embodiment 9 fully.
Comparative example 19
Use pure water to replace four (trimethylsiloxy group) silane of embodiment 9, other repeats embodiment 9 fully.
Comparative example 20
The color acceptance of embodiment 9 is increased to 1.3 times of (total amounts of pigment: 9.66 quality %), the amount of four (trimethylsiloxy group) silane is reduced to 13.54 quality %, in addition repeat embodiment 9 fully.
Comparative example 21
The color acceptance of embodiment 9 the is reduced to 1/4 (total amount of pigment: 9.55 quality %), the amount of four (trimethylsiloxy group) silane is increased to 53.65 quality %, in addition repeat embodiment 9 fully.
Each foundation cream is carried out following to the skin efficiency evaluation.
[to the skin efficiency evaluation]
Respectively ask 10 professional evaluation personnel (project difference, evaluation personnel repeat sometimes) to estimate to each assessment item according to the metewand shown in the following table, with overall assessment personnel's summation score as evaluation result.The mark height is then to the effectiveness height of assessment item.(full marks: 50 minutes).
The metewand of skin efficiency evaluation
Benchmark | Mark |
Experience the effect height and experience effect | 5 4 |
Experience effect 3 slightly
Only experience some effects 2
Impression is less than effect 1
Evaluation result is as follows.
| Sense that skin is affine is excellent | Adhere to and feel good | The cosmetic persistency is good | Skin does not have dry sensation when smearing | There is not greasy feeling |
Embodiment 9 | ◎ | ◎ | ◎ | ◎ | ◎ |
Embodiment 10 | ◎ | ◎ | ◎ | ◎ | ◎ |
Comparative example 10 | ◎ | ○ | ◎ | × | ○ |
Comparative example 11 | △ | △ | ○ | ◎ | × |
Comparative example 12 | × | × | × | ◎ | × |
Comparative example 13 | × | × | △ | ◎ | × |
Comparative example 14 | × | ○ | △ | ◎ | ○ |
Comparative example 15 | × | × | × | ◎ | ○ |
Comparative example 16 | ○ | △ | △ | ◎ | △ |
Comparative example 17 | △ | △ | △ | ◎ | × |
Comparative example 18 | × | × | × | × | △ |
Comparative example 19 | × | × | ○ | ◎ | ○ |
Comparative example 20 | × | × | △ | △ | × |
Comparative example 21 | ○ | ○ | ○ | ○ | △ |
The stability of each foundation cream is estimated according to following estimation of stability.
[estimation of stability]
The embodiment sample of according to the rules method preparation and comparative example sample were placed for 3 weeks in the temperature chamber of 0 ℃, 25 ℃ and 45 ℃, judge under any temperature, whether as seen to separate according to following metewand and condense, estimate storage stability thus.
Benchmark | Estimate |
Not having the cohesion of separation has a little separation cohesion that the cohesion of separation is arranged | ○ △ × |
The result is as shown in the table.
(preparation stability)
| Preparation stability |
Embodiment 9 embodiment 10 comparative examples 10 comparative examples 11 comparative examples 12 comparative examples 13 comparative examples 14 comparative examples 15 comparative examples 16 comparative examples 17 comparative examples 18 comparative examples 19 comparative examples 20 comparative examples 21 | ○ ○ ○ × △ △ × ○ △ × × × × × |
The result shows shown in the last table: embodiments of the invention are compared with comparative example, the affine sense of skin, sensation, resistance to water, anti-sebum, preparation stability excellence.Comparative example 10 is to use the situation of volatile cyclic 5 aggressiveness siloxanes, and the greasy feeling of embodiment, dry sensation are also excellent.Example when comparative example 11 is more use M4Q, but the oiliness sense is arranged, therefore estimate relatively poor.
Comparative example 12 is the examples when not using volatile solvent, and the oiliness sense is strong, and the sense of being clamminess is arranged, and feels relatively poor.Comparative example 14 is the examples when not using solid oil, and viscosity is low, and the problem of overflowing is from container arranged.Example when comparative example 15 is more use solid oils, preparation is hard, and the problem of caking is arranged.Example when comparative example 16 is less use surfactants, stability of formulation has problem.Comparative example 17 is examples of more use surfactant, and problem is arranged sensuously.Comparative example 18 is the examples when not using pure water, and the evaluation aspect stability, sensation is all relatively poor.Comparative example 19 is examples of more use pure water, harsh feeling occurs, and there is problem the sensation aspect.Comparative example 20 is the examples when increasing the combined amount of pigment, and the balance of preparation is destroyed, the evaluation inequality of sensation, stability.Comparative example 21 is the examples when reducing the combined amount of pigment, aspect sensation still can, can average out, but the balance of preparation is damaged, be difficult to take out from container, stability has problem.
Embodiment 11: anti-ultraviolet cosmetic backing material
With 50 quality % concentration a kind of silicones trimethylsiloxy group silicic acid is dissolved in four (trimethylsiloxy group) silane, the preparation lysate is according to the formulation anti-ultraviolet cosmetic backing material of following table.
(composition A) (%)
(1) titanium oxide microparticle 4 of siloxane treated
(2) methyl three (trimethylsiloxy group) silane 10
(3) four (trimethylsiloxy group) silane 15
(4) polyether modified siloxane
(chemical industry society of SHIN-ETSU HANTOTAI makes KF6017) 1
(composition B)
(5) zinc oxide fine particles 6 of siloxane treated
(6) perfluoralkyl phosphate
The yellowish pink painted Muscovitum of handling 0.5
(composition C)
(7) cross-linking type organopolysiloxane globular powder (elastomer) 4
(8) dimethyl polysiloxane (KF96A-6) 2
(9) fluoridize dimethiconol 1
(10) the trimethylsiloxy group silicate solution 6
(11) the p-methoxycinnamic acid monooctyl ester 3
(12) PFPE 0.5
(components D)
(13) ethanol 10
(14) pure water surplus
(15) Aloe extract 1
(16) the raspberry extract 1
(17) the Hibiscus syriacus L. extract 0.5
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
[method for making]
Step 1 is broken with the roller pulverizing with composition A, makes cream.
Step 2 simple mixing composition C fully pulverizes with mixer.
Step 3 is mixed composition B and composition C, fully disperses the back to add composition A, further fully mixes.
Step 4 then adds the components D of uniform dissolution, fully stirs, and advances container with the stainless shot filling then, obtains goods.
Comparative example 22
Use ring-type 6 aggressiveness volatile siloxanes to replace four (trimethylsiloxy group) silane, other repeats embodiment 11 fully.
Embodiment 12
Use four (trimethylsiloxy group) silane to replace methyl three (trimethylsiloxy group) silane, other repeats embodiment 11 fully.
Comparative example 23
Use methyl three (trimethylsiloxy group) silane to replace four (trimethylsiloxy group) silane, other repeats embodiment 11 fully.
Embodiment 13,14 and 15: daily skin whitener
According to following formulation skin whitener.Mixed solvent use four (trimethylsiloxy group) silane and methyl three (trimethylsiloxy group) silane are 1: 1 mixed solvent.
Embodiment | 13 | 14 | 15 |
(composition A), (%), (1) KF6017, (2) KF6026, (3) KF56, (4) KF995, (5) mixed solvent, (composition B), (6) glycerine, (7) dipropylene glycol, (8) methyl p-hydroxybenzoate, (9) ascorbic acid sodium sulfovinate, (10) NAP, (11) GABA, (12) apple extractants, (antioxidant), (13) sodium chloride, (14) spices, (15) pure water | 1-5 12 10 5 10 0.2 0.1 0.1 0.1 0.1 0.9 0.1 surplus | 1-5 3 19 5 10 0.2 0.1 0.1 0.1 0.1 0.9 0.1 surplus | 12 5-12 5 10 0.2 0.1 0.1 0.1 0.1 0.9 0.1 surpluses |
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 995 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): decamethylcyclopentaandoxane siloxanes (D5)
[method for making]
Step 1 with composition A 60 ℃ of heating for dissolving.
Step 2 with composition B 60 ℃ of heating for dissolving.
Step 3 is added composition A among the composition B to while stirring, and emulsifying mixes.
Step 4 then is cooled to 30 ℃ while stir, and is filled to and makes goods in the container.
Comparative example 24
Use ethanol to replace the mixed solvent of embodiment 14, in addition all repeat embodiment 14.
Comparative example 25
Use liquid paraffin,light to replace the mixed solvent of embodiment 15, in addition all repeat embodiment 15.
Comparative example 26
Use preparation in the preparation comparative example 1 contain 35% 1,1,1,5,5, four (trimethylsiloxy group) silane of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes replaces the mixed solvent of embodiment 15, in addition all repeats embodiment 15.
Comparative example 27
With prepare in the above-mentioned preparation comparative example contain 35% 1,1,1,5,5, four (trimethylsiloxy group) silane of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes and four (trimethylsiloxy group) silane mixture, obtain containing 5% 1,1,1,5,5, four (trimethylsiloxy group) silane of 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes replaces the mixed solvent of embodiment 15 with this, in addition all repeats embodiment 15.
Embodiment 16: sunscreen
According to following formulation sunscreen.The anti-ultraviolet composition adopts p-methoxycinnamic acid 2-ethyl hexyl ester, handles titanium oxide microparticle, handles zinc oxide fine particles, handles the titanellow microgranule, uses trimethylsiloxy group silicic acid as silicone resin.
Handle titanium oxide microparticle and use following material:, coat the titanium oxide microparticle that is coated by the aluminium silicate of mean diameter 17nm with the octyl group trimethoxy silane, 160 ℃ of heat treated with the covering amount of 8 quality %.Handle zinc oxide fine particles and use following material: with the covering amount of 3 quality %, coating mean diameter with methylhydrogenpolysi,oxane is the zinc oxide fine particles of the silica-treated of 50nm, 170 ℃ of heat treated.Handle the titanellow microgranule and use following material:, coat through titanium oxide microparticle silica-treated, doping iron, 130 ℃ of heat treated with methylhydrogenpolysi,oxane with the covering amount of 3 quality %.
(composition A) (%)
Handle titanium oxide microparticle 8.0
Four (trimethylsiloxy group) silane 9.0
Methyl three (trimethylsiloxy group) silane 3.0
(composition B)
Handle titanellow microgranule 0.8
Handle zinc oxide fine particles 12.0
(composition C)
3 D cross-linked type organopolysiloxane globular powder (elastomer) 1.0
Dimethiconol 6.0
Four (trimethylsiloxy group) silane 15.0
Trimethylsiloxy group silicic acid 6.0
P-methoxycinnamic acid 2-ethyl hexyl ester 10.0
(components D)
Ethanol 13.0
The pure water surplus
Aloe extract 0.5
Composition A is broken with the roller pulverizing, make cream.Simple mixing composition C fully pulverizes with mixer.Composition B and composition C are mixed, fully disperse the back to add composition A, further fully mix.The components D that then adds uniform dissolution fully stirs, and advances container with the stainless shot filling then, obtains goods.
Comparative example 28
Use straight chain shape tetramer volatile siloxane to replace four (trimethylsiloxy group) silane, other repeats embodiment 16 fully.
Embodiment 17
Use four (trimethylsiloxy group) silane to replace methyl three (trimethylsiloxy group) silane, other repeats embodiment 16 fully.
Comparative example 29
Use methyl three (trimethylsiloxy group) silane to replace four (trimethylsiloxy group) silane, other repeats embodiment 16 fully.
Embodiment 18: sunscreen (frost)
(composition) (%)
(1) methyl three (trimethylsiloxy group) silane 3.0
(2) four (trimethylsiloxy group) silane 17.0
(3) liquid paraffin 10.0
(4)KF6017 1.9
(5)KF6026 4.0
(6) the 4-tert-butyl group-4 '-methoxy dibenzoyl methylmethane 7.0
(7) chloro distearyl dimethyl ammonium 0.8
(8) vitamin E acetate 0.1
(9) ethanol 1.0
(10) terre verte 1.2
(11) antiseptic is an amount of
(12) spice is an amount of
(13) pure water surplus
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(8) and (11) heating are mixed.
B: with composition (9), (10) and (13) heating, homodisperse mixes.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (12) obtains sunscreen (frost).
Embodiment 19: sunscreen (frost)
(composition) (%)
(1) four (trimethylsiloxy group) silane 18.0
(2)KF56 2.0
(3) liquid paraffin 1.5
(4)KF6012 4.0
(5) p-methoxycinnamic acid octyl group ester 5.0
(6) 1,3 butylene glycol 4.0
(7) sodium chloride 1.0
(8) antiseptic is an amount of
(9) spice is an amount of
(10) pure water is an amount of
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: composition (1)-(6) heating is mixed.
B: with composition (7)-(9) and (11) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (10) obtains sunscreen (frost).
Embodiment 20: sunscreen (frost)
(composition) (%)
(1) four (trimethylsiloxy group) silane 16.5
(2) methyl three (trimethylsiloxy group) silane 1.0
(3)KP 545 12.0
(4) three isooctyl acid glyceride 5.0
(5) p-methoxycinnamic acid octyl group ester 6.0
(6)KSG 21 5.0
(7)KF6017 1.0
(8) oleophylic processing zinc oxide 20.0
(9) sodium chloride 0.5
(10) 1,3 butylene glycol 2.0
(11) antiseptic is an amount of
(12) spice is an amount of
(13) pure water surplus
KF 545 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): acrylic acid silica alkane copolymer resins/decamethylcyclopentaandoxane 30% solution
KSG 21 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): the polyether-modified methyl polysiloxane/dimethyl polysiloxane of cross-linking type
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
[preparation method]
A: add composition (3) in a part of composition (1), make it even, adding ingredient (8) disperses with ball mill.
B: in remaining composition (1), mix (2) and (4)-(7), uniform mixing.
C: composition (9)-(11) and (13) are mixed, dissolved.
D: add C in B, A and composition (12) are added in emulsifying, obtain sunscreen (frost).
Embodiment 21: sunscreen (astringent)
(composition) (%)
(1) methyl three (trimethylsiloxy group) silane 13.0
(2) four (trimethylsiloxy group) silane 1.0
(3)KF 615A 10.0
(4) squalane 1.5
(5) p-methoxycinnamic acid octyl group ester 3.0
(6) titanium TT0-S2 2.0
(7) poly methyl silsesquioxane 0.7
(8) 1,3 butylene glycol 10.0
(9) sodium chloride 2.0
(10) the L-proline 0.1
(11) the 2-Hydroxycaprylic acid 1.0
(12) 2 hydroxy propanoic acid 5.0
(13) sodium hydroxide is an amount of
(14) antiseptic is an amount of
(15) spice is an amount of
(16) pure water surplus
KF 615A (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=14.0)
Titanium TTO-S2 (manufacturing of the former industry of stone society): hydrophobization is handled the titanium oxide ultra micron
[preparation method]
A: with composition (8)-(16) uniform dissolution.
B: composition (1)-(5) are mixed, add composition (6), (7), make it even.
Embodiment 22: sunscreen (emulsion)
(composition) (%)
(1) four (trimethylsiloxy group) silane 25.0
(2) single isostearic acid two glyceride 1.5
(3) five isostearic acids ten glyceride 1.5
(4)KF 6012 0.5
(5) olive oil 1.0
(6) titanium oxide microparticle 7.0
(7) glycerol 5.0
(8) sodium chloride 1.5
(9) antiseptic is an amount of
(10) spice is an amount of
(11) pure water surplus
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: composition (1)-(5) heating is mixed homodisperse composition (6).
B: composition (7)-(9) and (11) heating are mixed.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (10) obtains sunscreen (emulsion).
Embodiment 23: sunscreen (emulsion)
(composition) (%)
(1) four (trimethylsiloxy group) silane 15.0
(2) ethanol 5.0
(3)KF 56 3.0
(4) single isostearic acid sorbitan ester 1.0
(5)KF 6012 0.5
(6) silicone resin 1.0
(7) p-methoxycinnamic acid octyl group ester 4.0
(8) titanium oxide microparticle 8.0
(9) Sorbitol 2.0
(10) sodium chloride 2.0
(11) antiseptic is an amount of
(12) spice is an amount of
(13) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
Silicone resin: [Me
3SiO
1/2]/[SiO
2] than 50% methyl three (trimethylsiloxy group) solution of silane that is 0.8 the netted chemical compound of siloxanes (trimethylsiloxy group silicic acid)
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: composition (1)-(7) heating is mixed, with composition (8) homodisperse.
B: composition (9)-(11) and (13) heating are mixed.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (12) obtains sunscreen (emulsion).
The evaluation result of the foregoing description 11-23 and comparative example 22-29 is as shown in the table.
| Non-stimulated when smearing to skin | It is good to smear sense | Use easily as the cosmetic backing material | It is not coarse to smear the back skin |
Zero antiultraviolet cosmetic backing material embodiment, 11 comparative examples, 22 embodiment, 12 comparative examples 23 0 days are with skin whitener embodiment 13 embodiment 14 embodiment 15 comparative examples 24 comparative examples 25 comparative examples 26 comparative examples 27 0 sun-screening agent embodiment 16 comparative examples 28 embodiment 17 comparative examples 29 embodiment 18 embodiment 19 embodiment 20 embodiment 21 embodiment 22 embodiment 23 | 46 42 46 45 44 43 42 10 11 10 10 39 18 43 44 44 44 41 39 42 39 | 43 34 37 35 41 42 41 19 29 10 10 37 20 33 30 38 41 40 39 40 42 | 45 35 46 40 40 44 40 10 13 10 10 39 12 37 32 38 43 40 44 41 41 | 50 44 50 36 48 49 48 40 48 10 10 43 26 46 33 47 46 44 40 48 46 |
This evaluation result shows: any assessment item of embodiments of the invention all shows excellent performance.Embodiment compares with comparative example, and not only dry sensation is few, and spreadability is good, has the wetness sensation of appropriateness, excellence aspect sensation.And the preventing ultraviolet effect excellence of embodiments of the invention.The result of comparative example 26,27 shows: 1,1,1,5,5, and 5-hexamethyl-3-trimethylsiloxy group-3-hydroxyl trisiloxanes is many, and then there is problem sensation aspect, safety aspect.By the result of comparative example 28 as can be known: straight chain shape volatile siloxane makes skin feel to stimulate perceptual difference.
Embodiment 24: tanned cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 12.0
(2) methyl three (trimethylsiloxy group) silane 3.0
(3)KF 96A-100 5.0
(4)KP-562 0.5
(5) the polyglycerol-modified siloxanes 2.2 of side chain silicone-type
(HLB=5)
(6)KF 6026 6.0
(7) Palmic acid 0.2
(8) para-amino benzoic acid dimethyl octyl group ester 0.5
(9) the 4-tert-butyl group-4 '-methoxy dibenzoyl methylmethane 0.5
(10) Kaolin 0.5
(11) iron oxide red 0.2
(12) iron oxide yellow 0.3
(13) iron oxide black 0.1
(14) Muscovitum 1.0 of coating titanium oxide
(15) the L-sodium glutamate 3.0
(16) 1,3 butylene glycol 5.0
(17) the two octadecyl Dimethyl Ammonium 0.1 of chlorination
(18) antioxidant is an amount of
(19) antiseptic is an amount of
(20) spice is an amount of
(21) pure water surplus
KF 96A-100 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 100mm
2The dimethyl polysiloxane of/s
KP-562 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): mountain Yu base modified acroleic acid silicone grafted copolymer
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: with composition (1)-(9) and (18)-(19) heating for dissolving.
B: with composition (17) and a part (21) heated and stirred, dispersion treatment is carried out in adding ingredient (10)-(14) then.
C:, mix with B with the remainder uniform dissolution of composition (15)-(16) and (21).
D: stir down, in A, slowly add C, emulsifying, cooling, adding ingredient (20) obtains tanned cream.
The above-mentioned as can be known tanned cream that obtains does not have with the separation of temperature or time or the variations such as cohesion of powder, excellent in stability, and spreadability is good, has the wetness sensation of appropriateness.
Embodiment 25: foundation cream
(composition) (%)
(1) methyl three (trimethylsiloxy group) silane 30.0
(2) four (trimethylsiloxy group) silane 15.0
(3)KF 96A-6 5.0
(4)KF 6017 1.5
(5)KF 6026 0.5
(6) octadecyl dimethyl benzyl ammonium salt modified montmorillonite used 4.0
(7) hydrophobization is handled titanium oxide * 10.0
(8) hydrophobization is handled Talcum * 6.0
(9) hydrophobization is handled Muscovitum * 6.0
(10) hydrophobization is handled iron oxide red * 1.6
(11) hydrophobization is handled iron oxide yellow * 0.7
(12) hydrophobization is handled iron oxide black * 0.2
(13) dipropylene glycol 5.0
(14) methyl parahydroxybenzoate 0.3
(15) 2-amino-2-methyl-1, ammediol 0.2
(16) hydrochloric acid 0.1
(17) spice is an amount of
(18) pure water surplus
KF 96A-100 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 100mm
2The dimethyl polysiloxane of/s
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
*: hydrophobization is handled powder: the methylhydrogenpolysi,oxane of interpolation 2% in powder, carry out the heat treated gained then.
(preparation method)
A: composition (1)-(6) heating is mixed, and adding ingredient (7)-(12) make it even.
B: with composition (13)-(16) and (18) heating for dissolving.(pH of water system is 9.0).
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (17) obtains foundation cream.
The foundation cream that obtains does not as mentioned above not separate with temperature or time or the variations such as cohesion of powder, and not only excellent in stability, and cosmetic persistency is good.
Embodiment 26: foundation cream
(composition) (%)
(1)KF 96A-6 5.0
(2) four (trimethylsiloxy group) silane 4.0
(3) methyl three (trimethylsiloxy group) silane 11.0
(4) squalane 4.0
(5) two sad DOPCP 3.0
(6) myristic acid isostearic acid two glyceride 2.0
(7) α-single iso stearyl glyceryl ether 1.0
(8)KF 6015 1.0
(9) aluminium distearate salt 0.2
(10) hydrophobization is handled titanium oxide * 5.0
(11) hydrophobization is handled sericite * 2.0
(12) hydrophobization is handled Talcum * 3.0
(13) hydrophobization is handled iron oxide red * 0.4
(14) hydrophobization is handled iron oxide yellow * 0.7
(15) hydrophobization is handled iron oxide black * 0.1
(16) magnesium sulfate 0.7
(17) glycerol 3.0
(18) antiseptic is an amount of
(19) spice is an amount of
(20) pure water surplus
KF 6015 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.5)
*: hydrophobization is handled powder: powder is carried out 2% stearic acid handle gained
[preparation method]
A: composition (1)-(9) heating is mixed, and adding ingredient (10)-(15) make it even.
B: with composition (16)-(18) and (20) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (19) obtains foundation cream.
The foundation cream that obtains does not as mentioned above not separate with temperature or time or the variations such as cohesion of powder, and not only excellent in stability, and cosmetic persistency is good.
Embodiment 27: foundation cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 15.0
(2) methyl three (trimethylsiloxy group) silane 3.0
(3)KF 56 5.0
(4) single isostearic acid sorbitan ester 0.5
(5) single isostearic acid two glyceride 0.5
(6)KF 6012 1.0
(7) p-methoxycinnamic acid octyl group ester 3.0
(8) titanium oxide 10.0
(9) iron oxide red 0.13
(10) iron oxide yellow 0.3
(11) iron oxide black 0.07
(12) Talcum 2.5
(13) Sorbitol 2.0
(14) magnesium sulfate 0.1
(15) ethanol 10.0
(16) antiseptic is an amount of
(17) spice is an amount of
(18) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: with composition (8)-(12) uniform mixing.
B: composition (1)-(7) and (16) heating are mixed, add A, homodisperse mixes.
C: heated in composition (13)-(14) and (18), add among the B and emulsifying, cooling, adding ingredient (15) and (17) obtain foundation cream.
The foundation cream emulsified state that obtains as mentioned above is good, and not too temperature influence can not separate or condense in time, and stability is very excellent.
Embodiment 28: foundation cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 15.0
(2)KF 96A-6 5.0
(3) liquid paraffin 3.0
(4)KF 6015 3.0
(5) Palmic acid 0.5
(6)アエロジルRY20 5.0
(7) titanium oxide 6.0
(8) iron oxide red 0.25
(9) iron oxide yellow 0.6
(10) iron oxide black 0.12
(11) sericite 8.03
(12) dipropylene glycol 10.0
(13) magnesium sulfate 2.0
(14) antiseptic is an amount of
(15) antioxidant is an amount of
(16) spice is an amount of
(17) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6015 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.5)
ア エ ロ ジ Le RY200 (Japanese ァ ェ ロ ジ Le company make): hydrophobized silica
(preparation method)
A: with composition (7)-(12) uniform mixing.
B: composition (1)-(6) and (16) are mixed 70 ℃ of heating, add A, homodisperse mixes.
C: heated at 70 ℃ in composition (13)-(15) and (18), add among the B and emulsifying, cooling, adding ingredient (17) obtains foundation cream.
The emulsified state of the foundation cream that obtains as mentioned above as can be known is good, the cosmetic excellent durability, and temperature influence not too, stability in time is very excellent.
Embodiment 29: foundation cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 9.0
(2) decamethylcyclopentaandoxane 3.0
(5) methyl three (trimethylsiloxy group) silane 3.0
(6)KF 96A-6 8.0
(7) p-methoxycinnamic acid octyl group ester 3.0
(8) the 12-hydroxy stearic acid 1.0
(9)FL-100 15.0
(10)FPD-6131 5.0
(11)KMP 590 3.0
(12) fluorine compounds are handled titanium oxide microparticle * 8.0
(13) fluorine compounds are handled mica titanium * 1.0
(14) fluorine compounds are handled titanium oxide * 5.0
(15) fluorine compounds are handled iron oxide red * 0.9
(16) fluorine compounds are handled iron oxide yellow * 2.0
(17) fluorine compounds are handled iron oxide black * 1.0
(18) ethanol 15.0
(19) glycerol 3.0
(20) magnesium sulfate 1.0
(21) antiseptic is an amount of
(22) spice is an amount of
(23) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
FL-100 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): trifluoro propyl methylsiloxane
FPD-6131 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene trifluoro propyl methyl polysiloxane copolymer (HLB=5.4)
KMP 590 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): spherical silicone resin powder
*: fluorine compounds are handled powder: form with 5% coating of perfluor alkyl ethide di(2-ethylhexyl)phosphate ethanolamine salt
[preparation method]
A: with composition (10)-(16) uniform mixing.
B: composition (1)-(9) are mixed 70 ℃ of heating, add A, homodisperse mixes.
C: heated at 40 ℃ in composition (17)-(20) and (22), slowly add among the B and emulsifying, cooling, adding ingredient (21) obtains liquid foundation cream.
The foundation cream that obtains as mentioned above can not change with temperature or time, and stability is very excellent.
Embodiment 30: foundation cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 27.0
(2)KF 56 3.0
(3) three isooctyl acid glyceride 10.0
(4)KF 6017 1.0
(5)KF 6026 1.0
(6) single isostearic acid polyglycerin ester 3.0
(7) hydrophobization is handled mixed-powder (annotating 1) 18.0
(8) iron oxide red 1.2
(9) iron oxide yellow 2.6
(10) iron oxide black 0.2
(11) 1,3 butylene glycol 7.0
(12) sodium chloride 0.5
(13) antiseptic is an amount of
(14) spice is an amount of
(15) pure water surplus
(annotating 1) hydrophobization is handled mixed-powder
A) the siloxane treated titanium oxide microparticle 8.0
B) the siloxane treated zinc oxide fine particles 4.0
C) the siloxane treated Talcum 3.0
D) the siloxane treated Muscovitum 3.0
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition a-d is mixed.
B: composition (1)-(6) are mixed, and the dissolving of heating is with composition (7)-(10) homodisperse.
C: composition (11)-(13) and (15) are mixed, be added to then and carry out emulsifying among the B.
D: cooling C, add composition (14), obtain foundation cream.
The foundation cream adhering sense excellence that obtains as mentioned above, (Ga り on the bodyguard) is glossy in dressing, and the cosmetic persistency is very excellent, can not change with temperature or time in addition, and stability is also excellent.
Embodiment 31: suppurative mastitis
(composition) (%)
(1) four (trimethylsiloxy group) silane 9.0
(2) methyl three (trimethylsiloxy group) silane 1.0
(3)KF 56 4.0
(4) squalane 5.0
(5) silicone resin 1.0
(6) glyceryl dioleate 2.0
(7)KF 6017 2.0
(8)KF 6026 4.0
(9) Sorbitol sodium sulfate 2.0
(10) sodium chondroitin sulfate 1.0
(11) hyaluronate sodium 0.5
(12) propylene glycol 3.0
(13) antiseptic 1.5
(14) vitamin E acetate 0.1
(15) antioxidant is an amount of
(16) spice is an amount of
(17) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
Silicone resin: [Me
3SiO
1/2]/[SiO
2] than 50% methyl three (trimethylsiloxy group) solution of silane that is 0.8 the netted chemical compound of siloxanes (trimethylsiloxy group silicic acid)
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
(preparation method)
A: composition (1)-(8) and (13)-(14) heating are mixed.
B: with composition (9)-(12) and (17) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (16) obtains suppurative mastitis.
The suppurative mastitis persistency that obtains as mentioned above is good, can not change with temperature or time, and stability is also excellent.
Embodiment 32: mascara
(composition) (%)
(1)KP 545 20.0
(2) Palmic acid/thylhexoic acid dextrin 8.0
(3) Tissuemat E 4.0
(4) Cera Flava 7.0
(5) lecithin 0.5
(6) methyl three (trimethylsiloxy group) silane surplus
(7) four (trimethylsiloxy group) silane 5.0
(8) Fancol ID 20.0
(9) ferrum oxide 5.0
(10)アエロジルRY200 3.5
(11) Talcum 10.0
KP 545 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): acrylic acid silica alkane copolymer resins/decamethylcyclopentaandoxane 30% solution
ア エ ロ ジ Le RY200 (Japanese ア エ ロ ジ Le company make): hydrophobized silica
[preparation method]
A: with composition (1)-(8) mixed dissolution.
B: composition (9)-(11) are added among the A, disperse with roller.
The mascara persistency that obtains as mentioned above is good, can not change with temperature or time, and stability is also excellent.
Embodiment 33: protective skin cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 20.0
(2) tricaprylin 10.0
(3)KF 6017 1.5
(4)KF 6026 4.0
(5) chlorination phenyl dimethyl stearyl ammonium 1.0
(6) 1,3 butylene glycol 10.0
(7) maltol 10.0
(8) saponite 1.5
(9) antiseptic is an amount of
(10) spice is an amount of
(12) pure water surplus
KF6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(5) and (9) heating are mixed.
B: with composition (6)-(8) and (11) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (10) obtains frost.
The white persistency that obtains as mentioned above is good, can not change with temperature or time, and stability is also excellent.
Embodiment 34: protective skin cream
Use methyl three (trimethylsiloxy group) silane (M3T) and four (trimethylsiloxy group) silane (M4Q) according to 1: 1 blended mixed solution as mixed solution.
(composition) (%)
(1) mixed solution 10.0
(2)KF 96A-6 5.0
(3) liquid paraffin 5.0
(4) water-dispersion type silicone elastomer globular powder 2.0
(5)KF 6017 3.0
(6)KF 6026 5.0
(7) sodium citrate 2.0
(8) 1,3 butylene glycol 5.0
(9) antiseptic is an amount of
(10) spice is an amount of
(11) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(5) heating is mixed.
B: with composition (6)-(9) and (11) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (10) obtains frost.
The frost that obtains as mentioned above has the wetness sensation of appropriateness, and persistency is good, can not change with temperature or time, and stability is also excellent.
Embodiment 35: protective skin cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 20.0
(2) liquid paraffin 5.0
(3)KF 615A 1.0
(4) L-magnesium L-ascorbyl-2-phosphate salt 3.0
(5) dipropylene glycol 5.0
(6) glycerol 5.0
(7) antiseptic is an amount of
(8) spice is an amount of
(9) pure water surplus
KF 615A (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=14.0)
[preparation method]
A: with composition (1)-(3) uniform mixing.
B: heated in composition (5)-(7), make it even.
C: uniform dissolution composition (4), (9).
D: stir down, in A, slowly add B, add C again, emulsifying, adding ingredient (8) obtains frost.
The frost that obtains as mentioned above is easy and skin is affine, can not change with temperature or time, and stability is also excellent.
Embodiment 36: protective skin cream
Use methyl three (trimethylsiloxy group) silane and four (trimethylsiloxy group) silane according to 7: 3 blended mixed solutions as mixed solution.
(composition) (%)
(1) mixed solution 20.0
(2)KF 56 5.0
(3)KF 6012 1.5
(4) dextrin fatty acid ester 1.0
(5) glycerol 5.0
(6) sodium chloride 1.0
(7) antiseptic is an amount of
(8) spice is an amount of
(9) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: composition (1)-(4) heating is mixed.
B: with (5)-(7) and (9) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (8) obtains frost.
The usability of the frost that obtains as mentioned above is very good.In addition, resistance to water, absorption of perspiration excellence, the cosmetic retentivity is good, can not change with temperature or time, and stability is also excellent.
Embodiment 37: protective skin cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 18.0
(2)KF 96A-100 2.0
(3) polypropylene glycol (3) myristyl ether 0.5
(4)KF 6017 1.4
(5)KF 6026 2.5
(6) hydrophobization is handled titanium oxide microparticle * 1.0
(7) glycerol 3.0
(8) 70% Sorbitols 5.0
(9) citric acid 25.0
(10) sodium chloride 0.6
(11) antiseptic is an amount of
(12) spice is an amount of
(13) 32% ammonia 4.5
(14) pure water surplus
KF 96A-100 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 100mm
2The dimethyl polysiloxane of/s
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
*: hydrophobization is handled titanium oxide microparticle: aluminium stearate is handled titanium oxide microparticle
[preparation method]
A: composition (1)-(5) and (12) are mixed, then blending constituent (6) and stirring.
B: with composition (7)-(11) and (13)-(14) uniform dissolution.
C: slowly add B in A, emulsifying obtains frost.
Although the frost that obtains as mentioned above contains a large amount of citric acids, the spreadability in smearing is good, can not change with temperature or time, and stability is also excellent.
Embodiment 38: protective skin cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 15.0
(2) decamethylcyclopentaandoxane 1.0
(3)KF 96A-6 4.0
(4)KF 6012 5.0
(5) POE (5) octyl group lauryl ether 1.0
(6) monostearate polyoxyethylene sorbitan ester (20E.O.) 0.5
(7)サンスフエアSZ-5 4.0
(8) the siloxane treated titanium oxide microparticle 5.0
(9) liquid paraffin 2.0
(10) macadimia nut oil 1.0
(11) Radix Scutellariae extract * 1.0
(12) Radix Gentianae extract * * 0.5
(13) ethanol 5.0
(14) 1,3 butylene glycol 2.0
(15) antiseptic is an amount of
(16) spice is an amount of
(17) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
サ Application ス Off エ ァ SZ-5 (manufacturing of Asahi Glass society): silicic acid anhydride is handled zinc oxide; The particle diameter of interior bag 50% zinc oxide is the silicon dioxide of 0.01-10 μ m;
*: Radix Scutellariae extract: with 50% 1,3 butylene glycol water extraction
*: Radix Gentianae extract: with 20% ethanol-water extraction
[preparation method]
A: composition (7)-(10) uniform mixing is disperseed.
B: composition (1)-(6) are mixed, add A.
C: composition (11)-(15) and (17) are mixed, add B then, emulsifying.
D: cooling C, add composition (16), obtain frost.
The white adhering sense excellence that obtains as mentioned above, dressing is glossy, and the cosmetic retentivity is very excellent, can not change with temperature or time in addition, and stability is also excellent.
Embodiment 39: the hands frost
(composition) (%)
(1) four (trimethylsiloxy group) silane 1.0
(2) methyl three (trimethylsiloxy group) silane 11.0
(3) alpha olefin oligomer 10.0
(4) silicone resin 5.0
(5)KF 6017 1.9
(6)KF 6026 4.0
(7) chloro distearyl dimethyl ammonium 0.8
(8) vitamin E acetate 0.1
(9) Macrogol 4000 1.0
(10) glycerol 10.0
(11) terre verte 1.2
(12) antiseptic is an amount of
(13) spice is an amount of
(14) pure water surplus
Silicone resin: [Me
3SiO
1/2]/[SiO
2] than 70% methyl three (trimethylsiloxy group) solution of silane that is 1.15 the netted chemical compound of siloxanes (trimethylsiloxy group silicic acid)
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(8) and (12) heating are mixed.
B: with (9)-(11) and (14) heating for dissolving.
C: stirring is slowly added B down in A, emulsifying, and cooling, adding ingredient (13) gets frost in one's hands.
The retentivity of filming of the hands frost that obtains as mentioned above is good, can not change with temperature or time in addition, and stability is also excellent.
Embodiment 40: the hands frost
(composition) (%)
(1) four (trimethylsiloxy group) silane 30.0
(2) liquid paraffin 10.0
(3) amino modified silicone rubber 15.0
(4)KF 6017 4.0
(5) chloro distearyl dimethyl ammonium 0.8
(6) acetic vitamin B 0.1
(7) Macrogol 4000 1.0
(8) glycerol 10.0
(9) terre verte 1.2
(10) antiseptic is an amount of
(11) spice is an amount of
(12) pure water surplus
Amino modified silicone rubber: amine equivalent 70000g/mol
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
[preparation method]
A: with composition (1), (3) heating mixed dissolution, heating adding ingredient (2), (4)-(6), (10).
B: composition (7)-(9) and (12) heating are mixed.
C: in A, slowly add B, after the emulsifying, cooling, adding ingredient (11) gets frost in one's hands.
The hands frost that obtains as mentioned above can effectively be protected the people's who is engaged in the work of scrubbing skin, and temperature stability is very excellent.
Embodiment 41: hands frost (O/W)
(composition) (%)
(1)KP 545 5.0
(2) four (trimethylsiloxy group) silane 4.5
(3) methyl three (trimethylsiloxy group) silane 0.5
(4)KSG 16 2.5
(5) alpha olefin oligomer 5.0
(6) vaseline 5.0
(7) three isooctyl acid glyceride 3.0
(8)KF 6017 0.5
(9) single oleic acid polyoxyethylene sorbitan ester 1.0
(10)セピゲル305 2.0
(11) 1,3 butylene glycol 5.0
(12) glycerol 5.0
(13) antiseptic is an amount of
(14) spice is an amount of
(15) pure water surplus
KP 545 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): acrylic acid silica alkane copolymer resins/decamethylcyclopentaandoxane 30% solution
KSG 16 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): cross-linking type dimethyl polysiloxane/dimethyl polysiloxane
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
セ ピ ゲ Le 305: light liquid isoparaffin (manufacturing of SEPPIC company)
[preparation method]
A: with composition (1)-(8) uniform mixing.
B: with composition (9)-(12) and (14) uniform mixing.
C: add B and emulsifying in A, adding ingredient (13) obtains O/W hands frost.
The adhering sense excellence of the hands frost that obtains as mentioned above, dressing is glossy, and the cosmetic retentivity is very excellent, and is very excellent with the stability of temperature or time.
Embodiment 42: hands frost (O/W)
(composition) (%)
(1)KP 545 5.0
(2) four (trimethylsiloxy group) silane 4.0
(3) decamethylcyclopentaandoxane 1.0
(4)KP 561 8.0
(5) spermol 1.0
(6) three glyceryl isostearates 5.0
(7) stearic acid 3.0
(8) glyceryl monostearate 1.5
(9)KF 6015 0.7
(10) sesquialter oleic acid sorbitan ester 0.5
(11) single oleic acid polyoxyethylene sorbitan ester 1.0
(12) sodium hydroxide (1% aqueous solution) 10.0
(13) 1,3 butylene glycol 5.0
(14) antiseptic is an amount of
(15) spice is an amount of
(16) pure water surplus
KP 545 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): acrylic acid silica alkane copolymer resins/decamethylcyclopentaandoxane 30% solution
KF 6015 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.5)
KP 561 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): acrylic acid silica alkane copolymer resins: stearyl modification acrylate siloxanes
[preparation method]
A: composition (1)-(10) are mixed heating for dissolving.
B: composition (11)-(13) and (15) are mixed, heated.
C: in A, add B and emulsifying, cooling, adding ingredient (14) obtains O/W hands frost.
The adhering sense excellence of the hands frost that obtains as mentioned above, dressing is glossy, and the cosmetic retentivity is very excellent, and is very excellent with the stability of temperature or time.
Embodiment 43: moisturiser
(composition) (%)
(1) four (trimethylsiloxy group) silane 5.0
(2) methyl three (trimethylsiloxy group) silane 5.0
(3)KF 56 3.0
(4) liquid paraffin 5.0
(5) four-2 ethyl hexanoic acid pentaerythritol esters 3.0
(6) the 2 ethyl hexanoic acid cetyl ester 5.0
(7)KF 6017 1.0
(8)KMP 594 2.5
(9)アエロジルR972 2.0
(10) zinc stearate 2.0
(11) vitamin E acetate 3.0
(12) PEG400 1.0
(13) sodium lactate 1.0
(14) 1,3 butylene glycol 5.0
(15) antiseptic is an amount of
(16) spice is an amount of
(17) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KMP 594 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): spherical silicone elastomer toner
ア エ ロ ジ Le R972 (Japanese ア エ ロ ジ Le society make): hydrophobized silica
[preparation method]
A:, add composition (8)-(9), homodisperse with composition (1)-(7) and (10)-(11) uniform mixing.
B: add composition (12)-(15) and (17), dissolving.
C: in A, slowly add B and emulsifying, cooling then, adding ingredient (16) obtains moisturiser.
The moisturiser spreadability that obtains as mentioned above is good, and wetness sensation is arranged, and the sense of not being clamminess does not change with temperature or time, and usability, stability are very excellent.
Embodiment 44: the back protective skin cream shaves
(composition) (%)
(1) methyl three (trimethylsiloxy group) silane 30.0
(2) four (trimethylsiloxy group) silane 5.0
(3)KF 6017 2.9
(4)KF 6026 5.0
(5) Polyethylene Glycol (molecular weight: 400) 5.0
(6) the L-sodium glutamate 2.0
(7) allantoin 0.1
(8) Aloe extract is an amount of
(9) ethanol 3.0
(10) antiseptic is an amount of
(11) antioxidant is an amount of
(12) spice is an amount of
(13) pure water surplus
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(4) are mixed heating for dissolving.
B: composition (5)-(11) and (13) are mixed, heated.
C: in A, add B and emulsifying, cooling, adding ingredient (12), the back protective skin cream obtains shaving.
The back protective skin cream that shaves that obtains as mentioned above can keep moist feeling after smearing, stability is also very excellent.
Embodiment 45: the eye Wrinkle eliminating cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 3.0
(2) methyl three (trimethylsiloxy group) silane 17.0
(3)KF7312 J 5.0
(4)KF 6017 2.0
(5)KF 6026 5.0
(6) sodium chondroitin sulfate 2.0
(7) sodium lactate 1.0
(8) glycerol 50.0
(9) antiseptic is an amount of
(10) antioxidant is an amount of
(11) spice is an amount of
(12) pure water surplus
KF 7312 J (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): silicone resin:
[Me
3SiO
1/2]/[SiO
2] than the 50% decamethylcyclopentaandoxane solution that is 0.8 the netted chemical compound of siloxanes (trimethylsiloxy group silicic acid)
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1)-(5) and (10) heating are mixed.
B: with composition (6)-(9) and (12) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (11) obtains the eye Wrinkle eliminating cream.
The retentivity of filming of the eye Wrinkle eliminating cream that obtains as mentioned above is good, can not change with temperature or time, and stability is also very excellent.
Embodiment 46: eye shadow cream
(composition) (%)
(1) four (trimethylsiloxy group) silane 12.0
(2) methyl three (trimethylsiloxy group) silane 3.0
(3)KF 96A-6 10.0
(4)KF 6012 2.0
(5) PEG (10) lauryl ether 0.5
(6) LL handles chromium oxide * * 6.2
(7) siloxane treated ultramarine * 4.0
(8) LL handles the Muscovitum * * 6.0 of coated titanium
(9) sodium chloride 2.0
(10) propylene glycol 8.0
(11) antiseptic is an amount of
(12) spice is an amount of
(13) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
*: siloxane treated: the methylhydrogenpolysi,oxane of interpolation 3%, heat treated gained then in powder
*: LL handles: the N with 5%
ε-lauroyl-L-lysine (aginomoto company makes ア ミ ホ-プ LL) coats processing to powder
[preparation method]
A: composition (1)-(5) are mixed adding ingredient (6)-(8), homodisperse.
B: uniform dissolution composition (9)-(11) and (13).
C: stir down, in A, slowly add B, emulsifying, adding ingredient (12) obtains eye shadow cream.
The eye shadow cream gloss that obtains as mentioned above is good, and the cosmetic retentivity is good, can not change excellent in stability with temperature or time.
Embodiment 47: eyeliner
(composition) (%)
(1) four (trimethylsiloxy group) silane 5.0
(2) methyl three (trimethylsiloxy group) silane 17.0
(3)KF 96A-6 5.0
(4) ホ ホ バ oil 2.0
(5)KF 6017 1.0
(6) siloxane treated iron oxide black (notes) 20.0
(7) ethanol 5.0
(8) antiseptic is an amount of
(9) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
(notes) siloxane treated iron oxide black: the methylhydrogenpolysi,oxane of interpolation 2% in iron oxide black, carry out the heat treated gained then.
[preparation method]
A: with composition (1)-(5) mixing of heating, adding ingredient (6), homodisperse.
B: the solvent components of heating (7)-(9).
C: stir down, slowly add B in A, emulsifying obtains eyeliner.
The eyeliner gloss that obtains as mentioned above is good, and the cosmetic retentivity is good, and dressing is survivable, can not change excellent in stability with temperature or time.
Embodiment 48: eyeliner
(composition) (%)
(1) four (trimethylsiloxy group) silane 32.0
(2)KF 96A-6 5.0
(3) the siloxane treated iron oxide black 20.0
(4) vitamin E acetate 0.2
(5) ホ ホ バ oil 2.0
(6) bentonite 3.0
(7)KF 6012 2.0
(8) ethanol 10.0
(9) 1,3 butylene glycol 10.0
(10) antiseptic is an amount of
(11) spice is an amount of
(12) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6012 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=7.0)
[preparation method]
A: composition (1)-(2), (4)-(7) are mixed, adding ingredient (3), uniform mixing disperses.
B: composition (8)-(10) and (12) are mixed.
C: in A, slowly add B, emulsifying, cooling then adds composition (11), obtains eyeliner.
The eyeliner gloss that obtains as mentioned above is good, and the cosmetic retentivity is good, and dressing is survivable, can not change excellent in stability with temperature or time.
Embodiment 49: antiperspirant
(composition) (%)
(1) methyl three (trimethylsiloxy group) silane 26.0
(2) four (trimethylsiloxy group) silane 4.0
(3)KF 6026 1.0
(4) single oleic acid polyoxyethylene sorbitan ester (20E.O.) 0.5
(5) glycinate 20.0 of tetrachlorohydrex aluminum zirconium
(6) pure water surplus
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
[preparation method]
A: composition (1) and (2) are mixed.
B: composition (4) is dissolved in (5), adds composition (3).
C: stir down, slowly add B in A, emulsifying obtains antiperspirant.
The antiperspirant spreadability that obtains as mentioned above is good, is not clamminess, and less turns white, and has salubrious usability, can not change with temperature or time simultaneously, and stability is also excellent.
Embodiment 50: antiperspirant
(composition) (%)
(1)KSG-21 20.0
(2)KSG-15 20.0
(3) four (trimethylsiloxy group) silane 10.0
(4) methyl three (trimethylsiloxy group) silane 20.0
(5) coordination compound 20.0 of tetrachlorohydrex aluminum zirconium and glycine
(6)KF 96A-6 10.0
KSG-21 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): the polyether-modified methyl polysiloxane/dimethyl polysiloxane of cross-linking type
KSG 15 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): the polyether-modified methyl polysiloxane/decamethylcyclopentaandoxane of cross-linking type
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
[preparation method]
A: with composition (1)-(4), composition (6) uniform mixing.
B: composition (5) is added A, mix and disperse.
The antiperspirant that obtains as mentioned above is not clamminess, and is highly stable with the variation of temperature or time yet.
Embodiment 51: the clear gel cosmetics
(composition) (%)
(1) four (trimethylsiloxy group) silane 10.0
(2)KF 615A 10.0
(3) 1,3 butylene glycol 10.0
(4) PEG400 9.0
(5) the 2-Hydroxycaprylic acid 1.0
(6) Sorbitol (70% aqueous solution) 10.0
(7) citric acid is an amount of
(8) sodium citrate is an amount of
(9) antiseptic is an amount of
(10) spice is an amount of
(11) pure water surplus
KF 615A (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=14.0)
[preparation method]
A: with composition (3)-(11) uniform dissolution.
B: composition (1)-(2) are mixed, make it even.
C: stir down, slowly add A in B, emulsifying obtains the clear gel cosmetics.
The clear gel cosmetics that obtain as mentioned above are easy and skin is affine, can not change with temperature or time, and stability is also excellent.
Embodiment 52: emulsion
(composition) (%)
(1) four (trimethylsiloxy group) silane 13.0
(2)KF 96A-6 6.0
(3) squalane 5.0
(4) two sad DOPCP 3.0
(5) α-single oil base glyceryl ether 1.0
(6)KF 6017 2.0
(7) aluminium distearate salt 0.2
(8) magnesium sulfate 0.7
(9) glycerol 5.0
(10) antiseptic is an amount of
(11) spice is an amount of
(12) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
(preparation method)
A: composition (1)-(7) heating is mixed.
B: with composition (8)-(10) and (12) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (11) obtains emulsion.
The emulsion low viscosity that obtains as mentioned above, the texture exquisiteness, spreadability is good, has the moist feeling or the soft sense of appropriateness, and the cosmetic retentivity is very good, can not change with temperature or time, and stability is also excellent.
Embodiment 53: emulsion
(composition) (%)
(1) four (trimethylsiloxy group) silane 11.0
(2) methyl three (trimethylsiloxy group) silane 4.0
(3)KF 96A-6 6.0
(4) squalane 5.0
(5) two sad DOPCP 3.0
(6) α-single oil base glyceryl ether 1.0
(7)KF 6026 1.5
(8)KF 6017 1.0
(9) aluminium distearate 0.2
(10) dextrin fatty acid ester 1.0
(11) magnesium sulfate 0.7
(12) glycerol 5.0
(13) antiseptic is an amount of
(14) spice is an amount of
(14) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 6026 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methylsiloxane polyoxypropylene oil base methylsiloxane dimethylsiloxane copolymer (HLB=4.7)
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
[preparation method]
A: composition (1)-(10) heating is mixed.
B: with composition (11)-(13) and (15) heating for dissolving.
C: stir down, in A, slowly add B, emulsifying, cooling, adding ingredient (14) obtains emulsion.
The emulsion that obtains as mentioned above has salubrious usability, can not change with temperature or time simultaneously, and stability is also excellent.
Embodiment 54: emulsion
(composition) (%)
(1) four (trimethylsiloxy group) silane 10.0
(2)KF 56 5.0
(3) squalane 5.0
(4) four-2 ethyl hexanoic acid pentaerythritol esters 5.0
(5)KF 6017 3.0
(6)KMP 594 2.0
(7)アェロジルR972 0.5
(8) magnesium ascorbyl phosphate 1.0
(9) sodium chloride 1.0
(10) Polyethylene Glycol 11,000 1.0
(11) propylene glycol 8.0
(12) antiseptic is an amount of
(13) spice is an amount of
(14) pure water surplus
KF 56 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): methyl phenyl silicone
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KMP 594 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): spherical silicone elastomer toner
ア ェ ロ ジ Le R972 (Japanese ア ェ ロ ジ Le society make): hydrophobized silica
[preparation method]
A:, add composition (5)-(6) homodisperse with composition (1)-(4) uniform mixing.
B: in composition (13), add composition (7)-(9) and dissolving, make composition (10), (11) more evenly, add then.
C: in A, slowly add B and emulsifying, cooling then, adding ingredient (12) obtains emulsion.
The emulsion spreadability that obtains as mentioned above is good, and the sense of not being clamminess has the soft sense of smearing, and does not change with temperature or time, and stability is very excellent.
Embodiment 55: beautifying liquid
(composition) (%)
(1) four (trimethylsiloxy group) silane 12.0
(2) three isooctyl acid glyceride 10.0
(3)KF 6017 2.0
(4)KSG 21 0.2
(5) glycerol 10.0
(6) magnesium ascorbyl phosphate salt 3.0
(7) sodium chloride 2.0
(8) antiseptic is an amount of
(9) spice is an amount of
(10) pure water surplus
KF 6017 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene methyl polysiloxane copolymer (HLB=4.6)
KSG 21 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): the polyether-modified methyl polysiloxane/dimethyl polysiloxane of cross-linking type
(preparation method)
A: composition (1)-(4) heating is mixed.
B: with composition (5)-(8) and (10) heating, uniform dissolution.
C: stir down, in A, slowly add B and emulsifying, cooling, adding ingredient (9) obtains beautifying liquid.
The affine sense of beautifying liquid that obtains as mentioned above and skin well in addition, does not change with temperature or time, and stability is also excellent.
Embodiment 56: deodorizer
(composition) (%)
(1) four (trimethylsiloxy group) silane 3.0
(2)KF 96A-6 4.0
(3)KF 615A 1.0
(4) propylene glycol 31.0
(5) triclosan 0.1
(6) glycerol 15.0
(7) antiseptic is an amount of
(8) spice is an amount of
(9) pure water surplus
KF 96A-6 (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): viscosity 6mm
2The dimethyl polysiloxane of/s
KF 615A (manufacturing of chemical industry society of SHIN-ETSU HANTOTAI): polyoxyethylene polyoxypropylene methyl polysiloxane copolymer (HLB=14.0)
[preparation method]
A: composition (1)-(3) are mixed.
B: composition (5) is dissolved in composition (4), composition (6)-(9) are mixed.
C: one side vigorous stirring A, Yi Bian add B, carry out emulsifying.
D: 65 parts of C, 35 parts of propellants (normal butane, iso-butane, propane mixture) are joined aerosol can, obtain deodorizer.
The deodorizer that obtains as mentioned above is not clamminess, and has excellent stability.
Embodiment 57: aerosol composition (convergence, deodorant)
(composition) (%)
(1) the siloxane treated Muscovitum 3.0
(2) ALCA 2.0
(3) isopropyl methyl phenol 0.3
(4) sesquialter oleic acid sorbitan ester 0.2
(5) isopropyl myristate 5.0
(6) four (trimethylsiloxy group) silane 5.0
(7) methyl three (trimethylsiloxy group) silane 1.0
(8) spice is an amount of
(9) propellant surplus
[preparation method]
A: composition (1)-(8) are mixed.
D: with A pack into aerosol can, filling component (9) then.
The odor-resistant result height of the aerosol composition of the present invention that obtains as mentioned above is not clamminess when smearing, and redispersibility is good, so usability is very excellent.