CN105496814A - 4D nail polish gel and application method thereof - Google Patents

4D nail polish gel and application method thereof Download PDF

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Publication number
CN105496814A
CN105496814A CN201510874038.6A CN201510874038A CN105496814A CN 105496814 A CN105496814 A CN 105496814A CN 201510874038 A CN201510874038 A CN 201510874038A CN 105496814 A CN105496814 A CN 105496814A
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nail polish
nail
glue
parts
composite
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CN105496814B (en
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赵明
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Hangzhou Lai Fan Network Technology Co Ltd
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Hangzhou Lai Fan Network Technology Co Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
    • A61K8/41—Amines
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26—Aluminium; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35—Ketones, e.g. benzophenone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37—Esters of carboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
    • A61K8/4973—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom
    • A61K8/498—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with oxygen as the only hetero atom having 6-membered rings or their condensed derivatives, e.g. coumarin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/55—Phosphorus compounds
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73—Polysaccharides
    • A61K8/736—Chitin; Chitosan; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8152—Homopolymers or copolymers of esters, e.g. (meth)acrylic acid esters; Compositions of derivatives of such polymers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/86—Polyethers
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/89—Polysiloxanes
    • A61K8/891—Polysiloxanes saturated, e.g. dimethicone, phenyl trimethicone, C24-C28 methicone or stearyl dimethicone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q3/00—Manicure or pedicure preparations
    • A61Q3/02—Nail coatings
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D498/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms
    • C07D498/12—Heterocyclic compounds containing in the condensed system at least one hetero ring having nitrogen and oxygen atoms as the only ring hetero atoms in which the condensed system contains three hetero rings
    • C07D498/16—Peri-condensed systems
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2351/00—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
    • C08J2351/08—Characterised by the use of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds

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  • Polymers & Plastics (AREA)
  • Cosmetics (AREA)

Abstract

The invention relates to a 4D nail polish gel and an application method of the 4D nail polish gel coordinated with an LED UV gel lamp. The 4D nail polish gel comprises materials of 11,14-Dioxa-2,9-diazaheptadec-16-enoicacid,4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl-1-oxo-2-propenyl)oxy]ethylester, a compound shown as the formula I in the description, acrylic oligomers, 1-hydroxycyclohexylphenylketone, bisphenyl phosphine oxide (2,4,6-trimethylbenzoyl) and the like. The nail polish gel has the base gel and sealing layer two-in-one effect, can be easily stripped in layer when being removed, is full in color and high in brightness, has excellent integration with nails, has better antibacterial performance, and is healthy and environment-friendly.

Description

A kind of 4D nail polish glue and using method thereof
Technical field
The present invention relates to cosmetics synthesis generation field, particularly relate to the using method of a kind of 4D nail polish glue and cooperated with LED nail lamp thereof.
Background technology
Nail polish glue is all a very welcome makeups product in the women of all age group, and the personage that likes to be beautiful is spread upon on fingernail, to fingernail can be made colourful; The nail polish glue brand existed in the market is various, very different.
Publication number is that the Chinese invention patent application of CN102908266A discloses a kind of Environmental-friendnail nail enamel and preparation method thereof, and described Environmental-friendnail nail enamel comprises emulsion, film former, aqueous, environmental protective mill base and deionized water; Wherein, the monomer that prepared by described emulsion comprises butyl acrylate, styrene, methacrylic acid and vinyl hydroxy silicone oil; Described initiator is azodiisobutyronitrile; Although this patent claims that its nial polish is environment-friendly type nial polish, true really not so.
Publication number is that the Chinese invention patent application of CN102552059A discloses a kind of low stimulation nial polish, and this nial polish based on alcohols solvent and alcohols film former, then is equipped with the additives such as thickening agent, suspending agent, plasticizer, paint box essence and is uniformly mixed and forms; But this nial polish has very strong zest, contact skin also has certain burn sense and injury.
Meanwhile, in prior art unexposed unsoundness environmental protection, easily to peel off or the nail polish glue torn.
Summary of the invention
The object of this invention is to provide a kind of 4D nail polish glue, it has quick solidifying and easily peels off or tear, and stable performance is water-fastness, has no irritating odor, health environment-friendly, also can reach the advantage of noresidue without water cleaning.
Above-mentioned technical purpose of the present invention is achieved by the following technical programs:
Be suitable for a 4D nail polish glue for LED illumination curing, comprise the component of following weight portion:
11,14-bis-of 38-45 part dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
The formula I of 0.02-0.04 part;
The acrylate quasi-oligomer of 25-29 part;
The 1-hydroxycyclohexyl phenyl ketone of 2.4-2.9 part;
Two phenyl phosphine oxides (2,4,6-trimethylbenzoyl) of 2.5-3.1 part;
The hydroxyethyl methylacrylate of 11-13 part;
1.1-1.4 the triethanolamine of part;
The laureth-21 of 0.7-0.8 part;
1.5-2.8 part Muscovitum;
Its compounds of formula I is shown below:
As preferably of the present invention, containing more than one the coloring agent in C117200 red 0.9-1.6 part, C15850 red 0.5-1 part, C177499 black 2.8-3.6 part, the yellow 0.15-0.22 part of C177492, the yellow 0.14-0.21 part of CN15985, the blue 1.03-1.35 part of C177510 or the white 2.15-2.65 part of C177891 in described nail polish glue.
As preferably of the present invention, containing being in harmonious proportion glue 6-8 part in described nail polish glue; Described mediation glue is made up of the component of following weight portion:
Polyacrylate-2-cross linked polymer 42-48 part; Benzophenone 7-10 part; Ethyl methacrylate 23-28 part; Polydimethylsiloxane 8-16 part; Trimethylolpropane triacrylate 10-15 part.
As preferably of the present invention, containing first composite regulator 7-9 part and second composite regulator 8-10 part in described nail polish glue;
Described first composite regulator comprises polyglycereol-2-three isostearate, glycerol and the AVC mixture that 1:3-4:1-2 in mass ratio forms; And
Described second composite regulator comprises two isooctadecanol malic acid fat, silylanizing Silicon stone and the PAROSOL 1789 mixture that 1:2-4:1-3 in mass ratio forms.
As preferably of the present invention, containing the 3rd composite regulator 4-6 part in described nail polish glue; The mixture that described 3rd composite regulator comprises the deacetylation chitosan of deacetylation at 70-80% of the composition of 1:0.5-0.8:1.3-1.7 in mass ratio, molecular weight is the daltonian oligosaccharide of 1800-2000 and DPnB.
As preferably of the present invention, the preparation method of described deacetylation chitosan is: by chitin 135-145 DEG C of heat treated 1-2h in mass concentration 40-50% alkali liquor, make deacetylation 70-80%, molecular weight is the daltonian chitosan of 20000-35000.
As preferably of the present invention, the preparation method of described polyacrylate-2-cross linked polymer is:
(1) prepared polymer P (MMA-MAh)-PEG600030-40 part, regulator solution 40-60 part form just mixed liquid by weight; Described regulator solution is comprise the carbonic allyl ester solution that sodium perchlorate that concentration is 0.4-0.7mol/L and concentration are the N-butyl benzimidazole of 0.3-0.8mol/L; MMA in described polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, MAh is maleic anhydride, P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, PEG6000 to be molecular weight be 6000 Polyethylene Glycol;
(2) in described just mixed liquid, add 2-7 part ten dihydroxystearic acid, be heated to 30-45 DEG C of reaction 5-9min under nitrogen protection;
(3) with obtaining polyacrylate-2-cross linked polymer after deionized water rinsing drying.
As preferably of the present invention, containing the 4th composite regulator 1-4 part in described nail polish glue;
Described 4th composite regulator is made up of the raw material of following parts by weight:
Spermol caprylate 28-33 part, 1,3-propanedicarboxylic acid 15-18 part, butantriol 8-10 part, Zinc Oxide 5-7 part, magnesium oxide 3-5 part, neoprene 18-23 part, elastic plastic 70-95 part, softening oil 2-3 part, DMC dimethyl carbonate 15-20 part and ethylbenzene 22-28 part;
Described elastic plastic comprises the first elastic plastic and the second elastic plastic that mix by weight 1:2-5;
The solids content that described first elastic plastic comprises 15-30 part weight is the emulsion acrylic resin of 60-75%, 12-15 part aqueous polyurethane, the acrylic resin powder of 5-8 part weight, the solids content of 2-6 part weight are the EVA emulsion of 20-35% and the chlorinated polypropylene of 1-4 part weight;
The preparation method of described second elastic plastic is: be that the polyvinyl alcohol water solution of 20-25% and the aqueous polyurethane aqueous solution of 20-30 part 15-20wt% are heated to 60-80 DEG C by 1-5 part mass concentration, the acrylate of 10-15 part is added after being cooled to 30-50 DEG C, then add the Lithium hydrate of 0.1-0.2 part and be warming up to 100-110 DEG C, add the sclerotin albumen of 5-8 part again, the Colophonium fat of 6-9 part, the eugenol of 2-4 part, and be cooled to 45-55 DEG C after insulation reaction 3-5 hour, then the bamboo charcoal micropowder of 6-8 part is added, the anion powder of 2-7 part and the OPEO of 10-13 part, stir 1-1.5 hour, cooling, obtained described second elastic plastic.
As preferably of the present invention, the preparation method of this kind of nail polish glue is: the following component of adding corresponding weight portion in order successively
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 10-15min, then add all described first composite regulators and continue to stir 3-6min; Then add whole described mediation glue and stir 5-9min, then add all described 4th composite regulators and continue to stir 2-5min; Finally add all described 3rd composite regulators to continue to stir 1-4min, obtain finished product.
As preferably of the present invention, the preparation method of described triethanolamine is:
(1) oxirane, ammonia are sent in reactor, at reaction temperature 36-38 DEG C, under reaction pressure 100-300kPa, carry out condensation reaction generate one, two, triethanolamine mixed liquor;
(2) at 100-110 DEG C through dewater concentrated after, sends into three vacuum rectification tower and carries out distilling under reduced pressure, by different boiling intercepting fraction, thus obtain triethanolamine semi-finished product;
(3) remove the removal of impurity with vapor distillation, and add sodium hydroxide and make triethanolamine become alkali metal salt and separate out, neutralization after being separated, then carry out distilling under reduced pressure and obtain triethanolamine sterling.
Another object of the present invention is to the using method that a kind of 4D nail polish glue cooperated with LED nail lamp is provided, comprise the steps:
(1) nail surface is cleaned;
(2) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface;
(3) frivolous on nail surface, evenly scribble one deck armor glue; In LED nail lamp, 60 seconds-120 seconds are irradiated to nail surface; This step according to demand or hobby can repeat 1-2 time;
(4) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface.
In sum, the present invention has following beneficial effect:
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl ester, with, acrylate quasi-oligomer, these two kinds of materials are main in nail polish glue of the present invention plays sizing colloid action.
1-hydroxycyclohexyl phenyl ketone, with two phenyl phosphine oxide (2,4,6-trimethylbenzoyl), these two kinds of materials mainly play light-sensitive emulsion effect in nail polish glue of the present invention, the stable light of nail polish glue can be kept beautiful, prevent xanthochromia; And nail polish glue of the prior art, the easy thinning jaundice of fingernail, and need to do in addition a maintenance, uneconomical.
Hydroxyethyl methylacrylate, mainly play solvent action in the present invention, simultaneously with the material 11 of specific deal, 14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl ester and acrylate quasi-oligomer, and the material common combination of all the other specified weight parts, can reach fast setting, therefore the present invention is particularly suitable for being irradiated by LED nail lamp, and general illumination 60 seconds just can film-forming; LED nail lamp is irradiated more of a specified duration, and persistence is higher; Meanwhile, the present invention is convenient to flood when removal and is easily divested.
The disadvantage that existing strippable water-soluble nail polish glue exists easily touches aquation to open, and nail polish glue of the present invention stable performance is water-fastness, also easily peels off or tear simultaneously, having no irritating odor, health environment-friendly; Form the film coating of light after dry, stable performance, and color is full, color and persistency good, at least can maintain above time in one to two week stands intact.
Triethanolamine and laureth-21, be conducive to improving nail polish glue moistening effect, make the more sparkling and crystal-clear water of nail polish glue bright.
Muscovitum, is conducive to the physics and the stable chemical performance that improve nail polish glue of the present invention, is beneficial to simultaneously and makes nail polish glue of the present invention have more glossiness.
Formula I is the native compound that the present inventor extracts from Folium Ginkgo, can be used for the invasion and attack preventing and treating fungus.
During for changing nail colour, only needing to tear after nail tip strip off, reaching the effect of throwing in week and changing in week, safety and Health very easy to use; During removal also without the need to unload first water and tinfoil parcel, also without the need to use manicure push except or file worn.
During nail polish glue removal of the present invention, flood easily divests; there is fingernail maintenance effect; for fragile fingernail, there is enhancing protective effect; fingernail layering easy fracture problem can be improved comprehensively; simultaneously nail polish glue of the present invention and nail surface amalgamation good; after being painted with, except the change of nail colour, feel comfortable just as not being coated with nail polish glue.
Polydimethylsiloxane of the present invention is a kind of organosilicon, has good chemical stability and physiologically active, is a kind of in the material of human body health environment-friendly; The effect of levelling agent, remover and defoamer is had concurrently in nail polish glue of the present invention.
The present invention is in harmonious proportion glue, has armor effect; After adding nail polish glue to, being beneficial to nail polish glue can rapid draing, and stable performance is water-fastness, is beneficial to simultaneously and peels off or tear, have no irritating odor, health environment-friendly, also can reach noresidue without water cleaning.
Coloring agent can reconcile into not same color by multiple collocation; And there is excellent wearability and richness, each women can select color according to the hobby of oneself, occasion, described nail polish glue is painted on fingernail, reaches the effect that armor manicure is two-in-one.
There is after first composite regulator proportioning of the present invention excellent dispersion, coagulate the soup and anti-wear and wear-resistant performance; There is after second composite regulator proportioning antioxidation and bright and clean function; Two kinds of composite regulators are combined and can reach synergistic function; According to the nail polish glue of proportioning composition of the present invention, have the performance of high temperature resistant (more than 38 DEG C) and low temperature resistant (less than-10 DEG C) concurrently, make the nail polish glue made can be used for multiple special occasions, such as hot seashore or the north of cold, retention is stablized.
Wherein, DPnB is dipropylene; The present invention the 3rd composite regulator has good film forming and abrasion resistance; Have active hydroxyl and amino in chitosan macromole, they have stronger chemical reaction ability, and give a lot of excellent chemical property of chitosan and physiologically active, the effect of being cross-linked with each other of oligomeric sugar layer and chitosan layer can prevent degradation of chitosan too fast; Three kinds of composite regulators are combined and can reach synergistic function; Meanwhile, chitosan can play synergistic function with the same polydimethylsiloxane with good physiologically active again.
Chitin is the natural macromolecular material extracted from the cell wall of the shell of the Crustacean such as shrimp, Eriocheir sinensis and bacterium, algae rudimentary plant is that occurring in nature is only second to cellulosic second largest biologically-derived resource, wide material sources, it is excellent Renewable resource, in the face of today that resource is day by day deficient, make full use of novel Renewable resource and become particularly important, chitin receives much concern because of its excellent performance and renewable; Chitin, chitosan and their derivant have good inhibitory action to microorganisms such as antibacterial, yeast, funguses.
Polyacrylate-2-the cross linked polymer adopting the present invention to prepare has excellent film property, hot property and dimensional stability, be beneficial to and make nail polish glue easily solidify under the illumination of LED nail lamp and easily peel off or tear, there is enough brightness, have no irritating odor, health environment-friendly, also can reach noresidue without water cleaning.
Adopt the 4th composite regulator of the present invention, there is the advantage that tack is good, fastness is high, add the 4th composite regulator, coordinate remaining specified weight serving matter, make nail polish glue of the present invention possess the two-in-one effect of primer sealing, and be beneficial to peelable tearable in use, have no irritating odor, health environment-friendly, also can reach noresidue without water cleaning.
Time prepared by nail polish glue mix and blend, the performance of order on product that various composition adds has impact; The nail polish glue prepared according to the inventive method order of addition is meeting under the requirement of easily peeling off or tearing, and is beneficial to and improves stability and wearability.
Therefore, the invention provides a kind of LED4D using method of health, its advantage mainly contains, and is also the 4D described in present subject matter, i.e. 4 primary efficacy, refers to:
1, nail polish glue of the present invention possesses the two-in-one effect of primer sealing;
2, nail polish glue of the present invention is coated in after on fingernail, and adopt LED nail lamp photocuring to be curable film-forming in general 60 seconds, persistency is good, and duration can reach 1-2 week; During removal without the need to unload first water and tinfoil parcel, also without the need to use manicure push except or file bar worn; During removal, flood easily divests, and has fingernail maintenance effect, has enhancing protective effect for fragile fingernail, can improve fingernail layering easy fracture problem comprehensively; Be convenient to the needs of satisfied different occasion different colours, have no irritating odor, health environment-friendly, also can reach noresidue without water cleaning;
3, nail polish glue of the present invention can present color thousand is that colourful, directly can refer to color use as colour, and have excellent wearability and richness, color is full, and light extremely, glitters very much; And nail polish glue of the present invention and fingernail have good amalgamation, after being painted with, except the change of nail colour, feel comfortable just as not being coated with nail polish glue;
4, there is no light trigger in formula of the present invention, there is no ethereal oil solvent, benzene, formaldehyde, ethyl acetate, DBP class harmful substance is not had yet, and there is environmental protection, quick-drying, light requirement is not according to, advantage that film forming is stable, and in formula of the present invention, with the addition of the formula I extracted from Folium Ginkgo, and the employing of chitin, chitosan and their derivant, there is good inhibitory action to microorganisms such as antibacterial, yeast, funguses; Therefore, health environment-friendly of the present invention, has no irritating odor, little to human injury's property, and has good armor effect.
Embodiment
Below by embodiment, the invention will be further described.The method described in the embodiment of the present invention that it should be understood that is only used for the present invention is described, instead of limitation of the present invention, under concept thereof of the present invention, all belong to the scope of protection of present invention to the simple modifications of preparation method of the present invention.The all raw materials used in embodiment and solvent are all purchased from SigmaBiochemicalandOrganicCompoundsforResearchandDiagnos ticClinicalReagents company.
The preparation embodiment of formula I:
Be raw material with Folium Ginkgo, pulverized and extract 2 ~ 4 times, each 12h ~ 72h by soak with ethanol, extracting solution merged, filtering and obtaining described Folium Ginkgo extract extractum after concentrating; Wherein ethanol: Folium Ginkgo=3 ~ 4:1, weight ratio.
Rear dry column-packing will be mixed with 60 ~ 120 order silica gel of 2 ~ 5 times of weight for described extractum after above-mentioned Folium Ginkgo extract extractum acetone solution, then gradient elution is carried out with grade chloroform-methanol solution that volume ratio is followed successively by 9:1,8:2,7:3,6:4,5:5, the eluent that collection obtains when being wherein the chloroform-methanol eluting of 9:1 by volume ratio, is called the first eluent; Above-mentioned first eluent silica gel column chromatography is continued to be separated, the chloroform-acetone solution being followed successively by 15:1,10:1,5:1,2:1 by volume ratio carries out gradient elution, and the eluent obtained when wherein volume is the chloroform-acetone solution eluting of 10:1 is called the second eluent; Above-mentioned second eluent silica gel column chromatography is continued to be separated, the petroleum ether-ethyl acetate solution being followed successively by 9:1,8:2,7:3,6:4,5:5 by volume ratio carries out gradient elution, and the eluent obtained when wherein volume ratio is the petroleum ether-ethyl acetate eluting of 7:3 is called the 3rd eluent.
Above-mentioned 3rd eluent is passed into high pressure liquid chromatography (pressure is at the reversed-phase preparative chromatography of 5-15Mpa) and carries out separation and purification, this high pressure liquid chromatography adopts 21.2mm × 250mm, the C of 5 μm 18chromatographic column, mobile phase is the methanol aqueous solution of 60wt%, flow rate of mobile phase is 12mL/min, UV-detector determined wavelength is 374nm, 3rd eluent each sample introduction 60 ~ 150 μ L, eluent corresponding when to collect chromatographic peak retention time after each sample introduction be 31min, namely obtains described formula I after desolvation
After obtaining above-mentioned formula I, again can be dissolved in methanol solution, and be mobile phase with methanol solution, carry out chromatography by gel column, described formula I of can purifying further.
Formula I is yellow powder; The key structural feature peak of the following ultraviolet spectra, infrared spectrum and the proton magnetic that list formula I.
Ultraviolet spectra (solvent is methanol): λ max(log ε) 210 (4.36), 266 (3.82), 374 (3.68) nm;
Infrared spectrum (pressing potassium bromide troche): v max3452,2924,2615,1668,1612,1516,1437,1316,1247,1182,1083,1022,868,722cm -1;
1HNMR(500MHz,CDCl 3,ppm)δ:10.7(s-OH),9.48(s-OH)6.28-7.52(d,-CH5H),6.57(s,1H),6.18(s1H),3.27(d,-CH 2),1.99-3.81(d,-CH 39H).
The preparation embodiment of nail polish glue:
Mediation glue formula 1: polyacrylate-2-cross-linked polymeric 48 parts; Benzophenone 10 parts; Ethyl methacrylate 28 parts; Polydimethylsiloxane 16 parts; Trimethylolpropane triacrylate 15 parts.
Mediation glue formula 2: polyacrylate-2-cross linked polymer 42 parts; Benzophenone 7 parts; Ethyl methacrylate 23 parts; Polydimethylsiloxane 8 parts; Trimethylolpropane triacrylate 10 parts.
Mediation glue formula 3: polyacrylate-2-cross linked polymer 45 parts; Benzophenone 8 parts; Ethyl methacrylate 26 parts; Polydimethylsiloxane 13 parts; Trimethylolpropane triacrylate 14 parts.
First composite regulator formula 1:
Polyglycereol-2-three isostearate, glycerol and AVC be 1:3:2 mixing composition in mass ratio.
First composite regulator formula 2:
Polyglycereol-2-three isostearate, glycerol and AVC be 1:4:1 mixing composition in mass ratio.
First composite regulator formula 3:
Polyglycereol-2-three isostearate, glycerol and AVC be 1:3:1 mixing composition in mass ratio.
Second composite regulator formula 1: two isooctadecanol malic acid fat, silylanizing Silicon stone and PAROSOL 1789 be 1:2:3 mixing composition in mass ratio.
Second composite regulator formula 2: two isooctadecanol malic acid fat, silylanizing Silicon stone and PAROSOL 1789 be 1:4:1 mixing composition in mass ratio.
Second composite regulator formula 3: two isooctadecanol malic acid fat, silylanizing Silicon stone and PAROSOL 1789 be 1:3:2 mixing composition in mass ratio.
3rd composite regulator formula 1: deacetylation is 1800 daltonian oligosaccharide and DPnB 1:0.5:1.7 mixing composition in mass ratio at deacetylation chitosan, the molecular weight of 70%.
3rd composite regulator formula 2: deacetylation is 2000 daltonian oligosaccharide and DPnB 1:0.8:1.3 mixing composition in mass ratio at deacetylation chitosan, the molecular weight of 80%.
3rd composite regulator formula 3: deacetylation is 1900 daltonian oligosaccharide and DPnB 1:0.6:1.5 mixing composition in mass ratio at deacetylation chitosan, the molecular weight of 75%.
4th composite regulator formula 1:
Spermol caprylate 28 parts, 1,3-propanedicarboxylic acid 15 parts, butantriol 8 parts, Zinc Oxide 5 parts, magnesium oxide 3 parts, neoprene 18 parts, elastic plastic 70 parts, softening oil 2 parts, DMC dimethyl carbonate 15 parts and 22 parts, ethylbenzene;
Elastic plastic comprises the first elastic plastic and the second elastic plastic that mix by weight 1:3;
The solids content that first elastic plastic comprises 15 parts of weight is the emulsion acrylic resin of 68%, 12 parts of aqueous polyurethanes, the acrylic resin powder of 5 parts of weight, the solids content of 2 parts of weight are the EVA emulsion of 29% and the chlorinated polypropylene of 1 part of weight.
4th composite regulator formula 2:
Spermol caprylate 33 parts, 1,3-propanedicarboxylic acid 18 parts, butantriol 10 parts, Zinc Oxide 7 parts, magnesium oxide 5 parts, neoprene 23 parts, elastic plastic 95 parts, softening oil 3 parts, DMC dimethyl carbonate 20 parts and 28 parts, ethylbenzene;
Elastic plastic comprises the first elastic plastic and the second elastic plastic that mix by weight 1:2;
The solids content that first elastic plastic comprises 30 parts of weight is the emulsion acrylic resin of 60%, the aqueous polyurethane of 15 parts of weight, the acrylic resin powder of 8 parts of weight, the solids content of 6 parts of weight are the EVA emulsion of 20% and the chlorinated polypropylene of 4 parts of weight.
4th composite regulator formula 3:
Spermol caprylate 30 parts, 1,3-propanedicarboxylic acid 16 parts, butantriol 9 parts, Zinc Oxide 6 parts, magnesium oxide 4 parts, neoprene 20 parts, elastic plastic 80 parts, softening oil 2.5 parts, DMC dimethyl carbonate 18 parts and 25 parts, ethylbenzene;
Elastic plastic comprises the first elastic plastic and the second elastic plastic that mix by weight 1:3;
The solids content that first elastic plastic comprises 20 parts of weight is the emulsion acrylic resin of 75%, 13 parts of aqueous polyurethanes, the acrylic resin powder of 7 parts of weight, the solids content of 4 parts of weight are the EVA emulsion of 35% and the chlorinated polypropylene of 2.5 parts of weight.
Embodiment one:
A kind of 4D nail polish glue comprises the component of following weight portion: 11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters 38 parts;
Formula I 0.02 part;
Acrylate quasi-oligomer 25 parts;
1-hydroxycyclohexyl phenyl ketone 2.4 parts;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl) 2.5 parts;
Hydroxyethyl methylacrylate 11 parts;
Triethanolamine 1.1 parts;
Laureth-210.7 parts;
1.5 parts, Muscovitum;
After above composition mixing, high-speed stirred mix homogeneously makes many effects 4D nail polish glue.
The preparation method of described triethanolamine is:
(1) oxirane, ammonia are sent in reactor, reaction temperature 36 DEG C, under reaction pressure 100kPa, carry out condensation reaction generate one, two, triethanolamine mixed liquor;
(2) at 100 DEG C through dewater concentrated after, sends into three vacuum rectification tower and carries out distilling under reduced pressure, by different boiling intercepting fraction, thus obtain triethanolamine semi-finished product;
(3) remove the removal of impurity with vapor distillation, and add sodium hydroxide and make triethanolamine become alkali metal salt and separate out, neutralization after being separated, then carry out distilling under reduced pressure and obtain triethanolamine sterling.
The using method of the present embodiment cooperated with LED nail lamp, comprises the steps:
(1) nail surface is cleaned;
(2) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface;
(3) frivolous on nail surface, evenly scribble one deck armor glue; In LED nail lamp, 60 seconds-120 seconds are irradiated to nail surface; This step according to demand or hobby can repeat 1-2 time;
(4) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface.
Embodiment two:
A kind of 4D nail polish glue comprises the component of following weight portion: 11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters 45 parts;
Formula I 0.04 part;
Acrylate quasi-oligomer 29 parts;
1-hydroxycyclohexyl phenyl ketone 2.9 parts;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl) 3.1 parts;
Hydroxyethyl methylacrylate 13 parts;
Triethanolamine 1.4 parts;
Laureth-210.8 parts;
2.8 parts, Muscovitum;
After above composition mixing, high-speed stirred mix homogeneously makes many effects 4D nail polish glue.
The preparation method of described triethanolamine is:
(1) oxirane, ammonia are sent in reactor, reaction temperature 38 DEG C, under reaction pressure 300kPa, carry out condensation reaction generate one, two, triethanolamine mixed liquor;
(2) at 110 DEG C through dewater concentrated after, sends into three vacuum rectification tower and carries out distilling under reduced pressure, by different boiling intercepting fraction, thus obtain triethanolamine semi-finished product;
(3) remove the removal of impurity with vapor distillation, and add sodium hydroxide and make triethanolamine become alkali metal salt and separate out, neutralization after being separated, then carry out distilling under reduced pressure and obtain triethanolamine sterling.
The using method of the present embodiment cooperated with LED nail lamp, comprises the steps:
(1) nail surface is cleaned;
(2) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface;
(3) frivolous on nail surface, evenly scribble one deck armor glue; In LED nail lamp, 60 seconds-120 seconds are irradiated to nail surface; This step according to demand or hobby can repeat 1-2 time;
(4) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface.
Embodiment three:
A kind of 4D nail polish glue comprises the component of following weight portion: 11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters 40 parts;
Formula I 0.03 part;
Acrylate quasi-oligomer 28 parts;
1-hydroxycyclohexyl phenyl ketone 2.7 parts;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl) 2.8 parts;
Hydroxyethyl methylacrylate 12 parts;
Triethanolamine 1.3 parts;
Laureth-210.8 parts;
2.5 parts, Muscovitum;
After above composition mixing, high-speed stirred mix homogeneously makes many effects 4D nail polish glue.
The preparation method of described triethanolamine is:
(1) oxirane, ammonia are sent in reactor, reaction temperature 37 DEG C, under reaction pressure 200kPa, carry out condensation reaction generate one, two, triethanolamine mixed liquor;
(2) at 105 DEG C through dewater concentrated after, sends into three vacuum rectification tower and carries out distilling under reduced pressure, by different boiling intercepting fraction, thus obtain triethanolamine semi-finished product;
(3) remove the removal of impurity with vapor distillation, and add sodium hydroxide and make triethanolamine become alkali metal salt and separate out, neutralization after being separated, then carry out distilling under reduced pressure and obtain triethanolamine sterling.
The using method of the present embodiment cooperated with LED nail lamp, comprises the steps:
(1) nail surface is cleaned;
(2) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface;
(3) frivolous on nail surface, evenly scribble one deck armor glue; In LED nail lamp, 60 seconds-120 seconds are irradiated to nail surface; This step according to demand or hobby can repeat 1-2 time;
(4) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface.
Embodiment four:
With the difference of embodiment one be, containing being in harmonious proportion 6 parts, glue, the first composite regulator 7 parts and the second composite regulator 8 parts in nail polish glue; Wherein, the first composite regulator is made according to the first composite regulator formula 1, and the second composite regulator is made according to the second composite regulator formula 1, and the glue that is in harmonious proportion is made according to mediation glue formula 1.
Prepared by nail polish glue: after adding the material in embodiment one, then adds all described second composite regulator stirring 10min, then adds all described first composite regulators and continues to stir 3min; Then add whole described mediation glue and stir 5min, obtain finished product.
As required, any one coloring agent in red 0.9 part of CI17200, red 5 parts of CI15850, yellow 0.15 part of black 2.8 parts of CI77499, CI77492, yellow 0.14 part of CI15985,1.03 parts, CI77510 indigo plant or white 2.65 parts of CI77891 can be added, make the nail polish glue with enough brightness of different colours.
Embodiment five:
With the difference of embodiment two be, containing being in harmonious proportion 8 parts, glue, the first composite regulator 9 parts and the second composite regulator 10 parts in nail polish glue; Wherein, the first composite regulator is made according to the first composite regulator formula 2, and the second composite regulator is made according to the second composite regulator formula 2, and the glue that is in harmonious proportion is made according to mediation glue formula 2.
Prepared by nail polish glue: after adding the material in embodiment one, then adds all described second composite regulator stirring 15min, then adds all described first composite regulators and continues to stir 6min; Then add whole described mediation glue and stir 9min, obtain finished product.
As required, any one coloring agent in red 0.9 part of CI17200, red 5 parts of CI15850, yellow 0.15 part of black 2.8 parts of CI77499, CI77492, yellow 0.14 part of CI15985,1.03 parts, CI77510 indigo plant or white 2.65 parts of CI77891 can be added, make the nail polish glue with enough brightness of different colours.
Embodiment six:
With the difference of embodiment three be, containing being in harmonious proportion 7 parts, glue, the first composite regulator 8 parts and the second composite regulator 9 parts in nail polish glue; Wherein, the first composite regulator is made according to the first composite regulator formula 3, and the second composite regulator is made according to the second composite regulator formula 3, and the glue that is in harmonious proportion is made according to mediation glue formula 3.
Prepared by nail polish glue: after adding the material in embodiment one, then adds all described second composite regulator stirring 15min, then adds all described first composite regulators and continues to stir 6min; Then add whole described mediation glue and stir 9min, obtain finished product.
As required, any one coloring agent in red 0.9 part of CI17200, red 5 parts of CI15850, yellow 0.15 part of black 2.8 parts of CI77499, CI77492, yellow 0.14 part of CI15985,1.03 parts, CI77510 indigo plant or white 2.65 parts of CI77891 can be added, make the nail polish glue with enough brightness of different colours.
Embodiment seven:
With the difference of embodiment four be, containing the 3rd composite regulator 4 parts in nail polish glue; Wherein, the preparation method of deacetylation chitosan is: by chitin 130 DEG C of heat treated 1h in mass concentration 40% alkali liquor, make deacetylation 70%, molecular weight is 20000 daltonian chitosans.Wherein, the 3rd composite regulator is made according to the 3rd composite regulator formula 1.
Preparation method is: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 12min, then add all described first composite regulators and continue to stir 4min; Then add whole described mediation glue and stir 7min, finally add all described 3rd composite regulators and continue to stir 3min, obtain finished product.
Embodiment eight:
With the difference of embodiment five be, containing the 3rd composite regulator 6 parts in nail polish glue; Wherein, the preparation method of deacetylation chitosan is: by chitin 150 DEG C of heat treated 2h in mass concentration 50% alkali liquor, make deacetylation 80%, molecular weight is 35000 daltonian chitosans.Wherein, the 3rd composite regulator is made according to the 3rd composite regulator formula 2.
Preparation method is: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 13min, then add all described first composite regulators and continue to stir 4min; Then add whole described mediation glue and stir 6min, finally add all described 3rd composite regulators and continue to stir 2min, obtain finished product.
Embodiment nine:
With the difference of embodiment six be, containing the 3rd composite regulator 5 parts in nail polish glue; Wherein, the preparation method of deacetylation chitosan is: by chitin 140 DEG C of heat treated 1.2h in mass concentration 45% alkali liquor, make deacetylation 78%, molecular weight is 25000 daltonian chitosans.Wherein, the 3rd composite regulator is made according to the 3rd composite regulator formula 3.
Preparation method is: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 11min, then add all described first composite regulators and continue to stir 5min; Then add whole described mediation glue and stir 7min, finally add all described 3rd composite regulators and continue to stir 3min, obtain finished product.
Embodiment ten:
With the difference of embodiment seven be, containing the 4th composite regulator 1 part in nail polish glue.Wherein, the 4th composite regulator is made according to the 4th composite regulator formula 1.
The preparation method of described second elastic plastic is: be that the polyvinyl alcohol water solution of 20% and the aqueous polyurethane aqueous solution of 20 parts of 15wt% are heated to 60 DEG C by 1 part of mass concentration, be cooled to the acrylate of interpolation 10 parts after 30 DEG C, then add the Lithium hydrate of 0.1 part and be warming up to 100 DEG C, add the sclerotin albumen of 5 parts again, the Colophonium fat of 6 parts, the eugenol of 2 parts, and insulation reaction was cooled to 45 DEG C after 3 hours, then the bamboo charcoal micropowder of 6 parts is added, the OPEO of the anion powder of 2 parts and 10 parts, stir 1 hour, cooling, obtained described second elastic plastic.
Prepared by nail polish glue: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 10min, then add all described first composite regulators and continue to stir 3min; Then add whole described mediation glue and stir 5min, then add all described 4th composite regulators and continue to stir 2min; Finally add all described 3rd composite regulators to continue to stir 1min, obtain finished product.
Wherein, the preparation method of the polyacrylate-2-cross linked polymer be in harmonious proportion in glue is:
(1) prepared polymer P (MMA-MAh)-PEG600030 part, regulator solution 40 parts form just mixed liquid by weight; Regulator solution is comprise the carbonic allyl ester solution that sodium perchlorate that concentration is 0.4mol/L and concentration are the N-butyl benzimidazole of 0.8mol/L; MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, PEG6000 to be molecular weight be 6000 Polyethylene Glycol;
(2) in first mixed liquid, add 2 part of ten dihydroxystearic acid, be heated to 30 DEG C of reaction 5-9min under nitrogen protection;
(3) with obtaining polyacrylate-2-cross linked polymer after deionized water rinsing drying.
Performance detects and obtains, the present embodiment has good resistance to water and adhesive force, and water absorption rate is lower than 3.2%; For the detection of traditional performance, as follows: with common coating method, coating as much as possible evenly; Be 32 DEG C in temperature, humidity is 50%, and sea water immersion is Sanya Yalongwan holiday resort sea water; All washings are general water-washing method, respectively simulation have a bath, go hands dirty, do housework, swimming etc., the suds of employing are general alkaline soap water, and detergent is regular powder, and this experiment adopts carves board.
After dry 20 minutes, under room temperature washing state, after 65 minutes, film is still without variable color, without coming off; Under 40 DEG C of warm water washing states, after 70 minutes, film is still without variable color, without coming off; Under suds washing state, after 30 minutes, film is still without variable color, without coming off; Under detergent washing state, after 60 minutes, film is still unchanged, without coming off; Under sea water immersion state, after 80 minutes, film is still without variable color, without coming off; Under accidental collision impact, film has and comes off.
Embodiment 11:
With the difference of embodiment eight be, containing the 4th composite regulator 4 parts in nail polish glue.Wherein, the 4th composite regulator is made according to the 4th composite regulator formula 2.
The preparation method of described second elastic plastic is: be that the polyvinyl alcohol water solution of 25% and the aqueous polyurethane aqueous solution of 30 parts of 20wt% are heated to 80 DEG C by 5 parts of mass concentrations, be cooled to the acrylate of interpolation 15 parts after 50 DEG C, then add the Lithium hydrate of 0.2 part and be warming up to 110 DEG C, add the sclerotin albumen of 8 parts again, the Colophonium fat of 9 parts, the eugenol of 4 parts, and insulation reaction was cooled to 55 DEG C after 5 hours, then the bamboo charcoal micropowder of 8 parts is added, the OPEO of the anion powder of 7 parts and 13 parts, stir 1.5 hours, cooling, obtained described second elastic plastic.
The preparation method of this nail polish glue is: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 15min, then add all described first composite regulators and continue to stir 6min; Then add whole described mediation glue and stir 9min, then add all described 4th composite regulators and continue to stir 5min; Finally add all described 3rd composite regulators to continue to stir 4min, obtain finished product.
Wherein, the preparation method of the polyacrylate-2-cross linked polymer be in harmonious proportion in glue is:
(1) prepared polymer P (MMA-MAh)-PEG600040 part, regulator solution 60 parts form just mixed liquid by weight; Regulator solution is comprise the carbonic allyl ester solution that sodium perchlorate that concentration is 0.7mol/L and concentration are the N-butyl benzimidazole of 0.3mol/L; MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, PEG6000 to be molecular weight be 6000 Polyethylene Glycol;
(2) in first mixed liquid, add 7 part of ten dihydroxystearic acid, be heated to 45 DEG C of reaction 9min under nitrogen protection;
(3) with obtaining polyacrylate-2-cross linked polymer after deionized water rinsing drying.
Performance detects and obtains, the present embodiment has good resistance to water and adhesive force, and water absorption rate is lower than 3.3%; For the detection of traditional performance, as follows: with common coating method, coating as much as possible evenly; Be 32 DEG C in temperature, humidity is 50%, and sea water immersion is Sanya Yalongwan holiday resort sea water; All washings are general water-washing method, respectively simulation have a bath, go hands dirty, do housework, swimming etc., the suds of employing are general alkaline soap water, and detergent is regular powder, and this experiment adopts carves board.
After dry 20 minutes, under room temperature washing state, after 70 minutes, film is still without variable color, without coming off; Under 40 DEG C of warm water washing states, after 75 minutes, film is still without variable color, without coming off; Under suds washing state, after 35 minutes, film is still without variable color, without coming off; Under detergent washing state, after 65 minutes, film is still unchanged, without coming off; Under sea water immersion state, after 85 minutes, film is still without variable color, without coming off; Under accidental collision impact, film has and comes off.
Embodiment 12:
With the difference of embodiment nine be, containing the 4th composite regulator 3 parts in nail polish glue.Wherein, the 4th composite regulator is made according to the 4th composite regulator formula 3.
The preparation method of described second elastic plastic is: be that the polyvinyl alcohol water solution of 23% and the aqueous polyurethane aqueous solution of 25 parts of 17wt% are heated to 70 DEG C by 2 parts of mass concentrations, be cooled to the acrylate of interpolation 12 parts after 40 DEG C, then add the Lithium hydrate of 0.2 part and be warming up to 105 DEG C, add the sclerotin albumen of 7 parts again, the Colophonium fat of 7 parts, the eugenol of 3 parts, and insulation reaction was cooled to 50 DEG C after 4 hours, then the bamboo charcoal micropowder of 7 parts is added, the OPEO of the anion powder of 6 parts and 12 parts, stir 1.2 hours, cooling, obtained described second elastic plastic.
The preparation method of this kind of nail polish glue is: add following component successively in order,
11,14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 12min, then add all described first composite regulators and continue to stir 5min; Then add whole described mediation glue and stir 6min, then add all described 4th composite regulators and continue to stir 3min; Finally add all described 3rd composite regulators to continue to stir 2min, obtain finished product.
Wherein, the preparation method of the polyacrylate-2-cross linked polymer be in harmonious proportion in glue is:
(1) prepared polymer P (MMA-MAh)-PEG600030-40 part, regulator solution 50 parts form just mixed liquid by weight; Regulator solution is comprise the carbonic allyl ester solution that sodium perchlorate that concentration is 0.6mol/L and concentration are the N-butyl benzimidazole of 0.4mol/L; MMA in polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, and MAh is maleic anhydride, and P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, PEG6000 to be molecular weight be 6000 Polyethylene Glycol;
(2) in first mixed liquid, add 5 part of ten dihydroxystearic acid, be heated to 35 DEG C of reaction 6min under nitrogen protection;
(3) with obtaining polyacrylate-2-cross linked polymer after deionized water rinsing drying.
Performance detects and obtains, the present embodiment has good resistance to water and adhesive force, and water absorption rate is lower than 3.1%; For the detection of traditional performance, as follows: with common coating method, coating as much as possible evenly; Be 32 DEG C in temperature, humidity is 50%, and sea water immersion is Sanya Yalongwan holiday resort sea water; All washings are general water-washing method, respectively simulation have a bath, go hands dirty, do housework, swimming etc., the suds of employing are general alkaline soap water, and detergent is regular powder, and this experiment adopts carves board.
After dry 20 minutes, under room temperature washing state, after 62 minutes, film is still without variable color, without coming off; Under 40 DEG C of warm water washing states, after 68 minutes, film is still without variable color, without coming off; Under suds washing state, after 33 minutes, film is still without variable color, without coming off; Under detergent washing state, after 61 minutes, film is still unchanged, without coming off; Under sea water immersion state, after 78 minutes, film is still without variable color, without coming off; Under accidental collision impact, film has and comes off.
Embodiment 13:
That the first composite regulator is made according to the first composite regulator formula 1 with the difference of embodiment ten; Second composite regulator is made according to the second composite regulator formula 2; 3rd composite regulator is made according to the 3rd composite regulator formula 3; 4th composite regulator is made according to the 4th composite regulator formula 1.
Embodiment 14:
That the first composite regulator is made according to the first composite regulator formula 1 with the difference of embodiment 11; Second composite regulator is made according to the second composite regulator formula 3; 3rd composite regulator is made according to the 3rd composite regulator formula 2; 4th composite regulator is made according to the 4th composite regulator formula 2.
Embodiment 15:
That the first composite regulator is made according to the first composite regulator formula 2 with the difference of embodiment 12; Second composite regulator is made according to the second composite regulator formula 1; 3rd composite regulator is made according to the 3rd composite regulator formula 3; 4th composite regulator is made according to the 4th composite regulator formula 3.
Activity experiment:
1, formula I activity experiment
Be suspended in MH culture medium by antibacterial (trichophyton, trichophyton gypseum and Epidermophvton trichophyton), dispersion concentration is approximately 10 5cfu ﹒ mL -1, being added to by bacterium liquid (every hole adds bacterium liquid 100 μ L) on 96 orifice plates, take culture medium as blank, replaces tested material as negative control, with itraconazole (Xian-Janssen Pharmaceutical Ltd.) for positive control using DMSO.Formula I is dissolved in DMSO and is made into 800,400,200,100,50,25 μ g ﹒ mL respectively -1solution is (for MIC 50be less than 5 μ g ﹒ mL -1, when carrying out a step experiment, the Concentraton gradient of preparation is 50,25,12.5,6.25,3.1,1.5 μ g ﹒ mL -1), join on 96 orifice plates with the amount of every hole 11 μ L that [ultimate density of medicinal liquid is respectively 80,40,20,10,5,2.5 μ gmL -1(be 5,2.5,1.25,0.63,0.31 and 0.15 μ gmL for the latter -1)], each Concentraton gradient does four parallel laboratory tests.The incubator that 96 orifice plates put into 37 DEG C is cultivated 24h, then every hole adds the PBS of the every mL of 25 μ L containing 4mgMTT, under similarity condition, cultivate 4h again, every hole adds 100 μ LSDS lysates (95mL tri-distilled water+10gSDS+5mL isopropyl alcohol+0.1mL concentrated hydrochloric acid) and cultivates 12h afterwards.Under 570nm, measure OD value by microplate reader, percent inhibition is calculated as follows:
Active height is with half suppression ratio MIC 50represent, MIC 50less, the activity of compound is higher, and result is: formula I is to trichophyton, trichophyton gypseum and Epidermophvton trichophyton half suppression ratio MIC 50be respectively 0.63,0.60 and 0.82; Itraconazole is to trichophyton, trichophyton gypseum and Epidermophvton trichophyton half suppression ratio MIC 50be respectively 0.63,0.70 and 0.65.
2, agent activity experiment:
Use preparation described in embodiment 1-5, carry out activity experiment as described below:
Cut about 0.5mm from the bight of Cornu Bovis seu Bubali thick, the small pieces of 1.5 × 3cm size also use embodiment 1-5 preparation process half side, once a day, and continuous five days.Then above the moisture agar surface this sheet being fixed on a moisture chamber about 0.5cm metal column on, the half side-view processed is down.The whole side of Cornu Bovis seu Bubali upward inoculates the microgonidium suspension of Trichophyton mentagrophytes in dots.Then, bacterium colony form is stored 10 days at 28 DEG C.
Adopt the pretreatment of the preparation of embodiment of the present invention 1-5 to prevent fungal spore for 5 times at half back side of Cornu Bovis seu Bubali to germinate at whole end face.Even after 90 days, still vaccination can not be observed at whole apical view under the microscope.Therefore, the embodiment 1-5 preparation containing formula I effectively can prevent conk.
According to the method described above, carry out control experiment, difference is that fungus has minority growing point on the Cornu Bovis seu Bubali side processed not containing formula I in preparation described in embodiment 1-5, but another half observed the good growth of fungus.
Do not adopt the blank of invention formulation process after inoculation, fungus is in the fully growth of Cornu Bovis seu Bubali surface.
When being coated on fingernail by nail polish glue of the present invention, health environment-friendly, has no irritating odor, and only needs to adopt the i.e. curable film-forming of LED light solidification illumination 1-2 minute, can rapid draing, forms the film coating of light, stable performance after dry; During for changing color, only need to tear after nail tip strip off, safety and Health very easy to use; Reach the effect of throwing in week and changing in week.During nail polish glue removal of the present invention, flood easily divests, and has fingernail maintenance effect, has enhancing protective effect for fragile fingernail, can improve fingernail layering easy fracture problem comprehensively.With the addition of the formula I extracted from Folium Ginkgo in formula of the present invention, effectively can prevent the generation of nail fungi.

Claims (10)

1. a 4D nail polish glue, is characterized in that the component comprising following weight portion:
11,14-bis-of 38-45 part dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl esters;
The formula I of 0.02-0.04 part;
The acrylate quasi-oligomer of 25-29 part;
The 1-hydroxycyclohexyl phenyl ketone of 2.4-2.9 part;
Two phenyl phosphine oxides (2,4,6-trimethylbenzoyl) of 2.5-3.1 part;
The hydroxyethyl methylacrylate of 11-13 part;
1.1-1.4 the triethanolamine of part;
The laureth-21 of 0.7-0.8 part;
1.5-2.8 part Muscovitum;
Described formula I is shown below:
2. nail polish glue according to claim 1, is characterized in that also containing more than one the coloring agent in C117200 red 0.9-1.6 part, C15850 red 0.5-1 part, C177499 black 2.8-3.6 part, the yellow 0.15-0.22 part of C177492, the yellow 0.14-0.21 part of CN15985, the blue 1.03-1.35 part of C177510 or the white 2.15-2.65 part of C177891.
3. nail polish glue according to claim 1, is characterized in that described mediation glue is made up of the component of following weight portion also containing being in harmonious proportion glue 6-8 part:
Polyacrylate-2-cross linked polymer 42-48 part; Benzophenone 7-10 part; Ethyl methacrylate 23-28 part; Polydimethylsiloxane 8-16 part; Trimethylolpropane triacrylate 10-15 part.
4. nail polish glue according to claim 3, is characterized in that in described nail polish glue containing first composite regulator 7-9 part and second composite regulator 8-10 part;
Described first composite regulator comprises polyglycereol-2-three isostearate, glycerol and the AVC mixture that 1:3-4:1-2 in mass ratio forms; And
Described second composite regulator comprises two isooctadecanol malic acid fat, silylanizing Silicon stone and the PAROSOL 1789 mixture that 1:2-4:1-3 in mass ratio forms.
5. nail polish glue according to claim 4, is characterized in that in described nail polish glue containing the 3rd composite regulator 4-6 part; The mixture that described 3rd composite regulator comprises the deacetylation chitosan of deacetylation at 70-80% of the composition of 1:0.5-0.8:1.3-1.7 in mass ratio, molecular weight is the daltonian oligosaccharide of 1800-2000 and DPnB.
6. nail polish glue according to claim 5, it is characterized in that, the preparation method of described deacetylation chitosan is: by chitin 135-145 DEG C of heat treated 1-2h in mass concentration 40-50% alkali liquor, make deacetylation 70-80%, molecular weight is the daltonian chitosan of 20000-35000.
7. nail polish glue according to claim 6, is characterized in that, the preparation method of described polyacrylate-2-cross linked polymer is:
(1) prepared polymer P (MMA-MAh)-PEG600030-40 part, regulator solution 40-60 part form just mixed liquid by weight; Described regulator solution is comprise the carbonic allyl ester solution that sodium perchlorate that concentration is 0.4-0.7mol/L and concentration are the N-butyl benzimidazole of 0.3-0.8mol/L; MMA in described polymer P (MMA-MAh)-PEG4000 is methyl methacrylate, MAh is maleic anhydride, P (MMA-MAh) is the copolymer of methyl methacrylate and maleic anhydride, PEG6000 to be molecular weight be 6000 Polyethylene Glycol;
(2) in described just mixed liquid, add 2-7 part ten dihydroxystearic acid, be heated to 30-45 DEG C of reaction 5-9min under nitrogen protection;
(3) with obtaining polyacrylate-2-cross linked polymer after deionized water rinsing drying.
8. nail polish glue according to claim 7, is characterized in that in described nail polish glue containing the 4th composite regulator 1-4 part;
Described 4th composite regulator is made up of the raw material of following parts by weight:
Spermol caprylate 28-33 part, 1,3-propanedicarboxylic acid 15-18 part, butantriol 8-10 part, Zinc Oxide 5-7 part, magnesium oxide 3-5 part, neoprene 18-23 part, elastic plastic 70-95 part, softening oil 2-3 part, DMC dimethyl carbonate 15-20 part and ethylbenzene 22-28 part;
Described elastic plastic comprises the first elastic plastic and the second elastic plastic that mix by weight 1:2-5;
The solids content that described first elastic plastic comprises 15-30 part weight is the emulsion acrylic resin of 60-75%, 12-15 part aqueous polyurethane, the acrylic resin powder of 5-8 part weight, the solids content of 2-6 part weight are the EVA emulsion of 20-35% and the chlorinated polypropylene of 1-4 part weight;
The preparation method of described second elastic plastic is: be that the polyvinyl alcohol water solution of 20-25% and the aqueous polyurethane aqueous solution of 20-30 part 15-20wt% are heated to 60-80 DEG C by 1-5 part mass concentration, the acrylate of 10-15 part is added after being cooled to 30-50 DEG C, then add the Lithium hydrate of 0.1-0.2 part and be warming up to 100-110 DEG C, add the sclerotin albumen of 5-8 part again, the Colophonium fat of 6-9 part, the eugenol of 2-4 part, and be cooled to 45-55 DEG C after insulation reaction 3-5 hour, then the bamboo charcoal micropowder of 6-8 part is added, the anion powder of 2-7 part and the OPEO of 10-13 part, stir 1-1.5 hour, cooling, obtained described second elastic plastic.
9. nail polish glue according to claim 8, it is characterized in that the preparation method of described nail polish glue is: the following substances 11 of adding corresponding weight portion in order successively, 14-bis-dislikes-2,9-diaza heptadecane-16-olefin(e) acid-4,4,6,16-tetramethyl-10,15-dioxo-2-[(2-methyl isophthalic acid-oxo-2-acrylic) oxo] ethyl ester;
Formula I;
Acrylate quasi-oligomer;
1-hydroxycyclohexyl phenyl ketone;
Two phenyl phosphine oxide (2,4,6-trimethylbenzoyl);
Hydroxyethyl methylacrylate;
Triethanolamine;
Laureth-21;
Muscovitum;
High-speed stirred mix homogeneously after above composition mixing, then add all described second composite regulator stirring 10-15min, then add all described first composite regulators and continue to stir 3-6min; Then add whole described mediation glue and stir 5-9min, then add all described 4th composite regulators and continue to stir 2-5min; Finally add all described 3rd composite regulators to continue to stir 1-4min, obtain finished product.
10. the using method of the arbitrary described 4D nail polish glue of claim 1-9, is characterized in that comprising the steps:
(1) nail surface is cleaned;
(2) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface;
(3) frivolous on nail surface, evenly scribble one deck armor glue; In LED nail lamp, 60 seconds-120 seconds are irradiated to nail surface; This step according to demand or hobby can repeat 1-2 time; (4) frivolous on nail surface, uniform application one deck diamond armor glue; LED nail lamp is used to irradiate 60 seconds-120 seconds to nail surface.
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