CN104693840B - Environment-friendly type nano coloring material aqueous dispersions and preparation method thereof - Google Patents
Environment-friendly type nano coloring material aqueous dispersions and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of environment-friendly type nano coloring material aqueous dispersions and preparation method thereof, its component of environment-friendly type nano coloring material aqueous dispersions includes: water, alhpa olefin sodium sulfonate and the copolymer of other monomer and dyestuff.The alhpa olefin sodium sulfonate that the present invention uses is the polymerizability or reactive emulsifier that a kind of activity is higher, and the existing emulsifiability of this emulsifying agent, is again the monomer that a kind of activity is higher, can be copolymerized with other monomer.By hydrophobic dye being dissolved in inside certain monomer during the nano-coloring material that the present invention provides, after polymerization, preparing the coloured polymer aqueous dispersion of nano-scale, the most this nano-coloring material has excellent storage stability in aqueous phase.
Description
Technical field
The present invention relates to a kind of environment-friendly type nano coloring material aqueous dispersions and preparation method thereof, particularly a kind of containing α-alkene
Hydrocarbon sulfonate sodium polymerisable emulsifier component be applicable to high performance hydrate colour ink-jet printing ink and be applied to make liquid
The colored filter mill base of crystal display, and high-grade paint, the nano-coloring material of the coloring agent of cosmetics etc..
Background technology
Nano-coloring material is that a kind of dyestuff is disperseed and to be fixed on the nanometer formed in nano-level crosslinked polymer particle multiple
Condensation material, is proposed in late 1990s at first by the research worker of Germany BASF, and in using miniemulsion to gather at the beginning of 21 century
Synthesis merit prepares [ClemensT, BoehmAJ, BayerSK.PolymerPreprint, 2000,41 (1): 24-25], and this is combined
Thing combines the performance of pigment and dyestuff, has excellent coloring, is prone to processing and durability.
Barashkov of RadiantColor company of the U.S. et al. uses encapsulation technology (Dye-
PackingTechnology, DPT), a kind of traditional emulsion polymerisation process is little for water miscible fluorescent dye mean diameter
Polymer particle in 140nm wires up, be prepared for a kind of aqueous jet printing fluorescence nano colorant (BarashkovNN,
IjuRH.InternationalConferenceonDigitalPrintingTechnologies,FortLauderdale,
2001,878-880), the colorant obtained has good water-fast, light resistance.But this method emulsifier is big, size tunable
The deficiency such as property is poor, dye content is low.
Hu Zhenkun etc. (patent documentation CN200610118671.3) use the mini-emulsion polymerization improved to be prepared for nano-coloring material,
Initially with the mini-emulsion polymerization reaction improved, the fixing of dye is obtained prepolymer seeds in cross linked polymer Nano microsphere, connect
And utilize involucrum polymerization technique to build modification, the shell of protectiveness at the surface of the seed.Nano-coloring material prepared by the method
Particle poor dispersion, and particle diameter wider distribution.
[Lelu S, Novat C, Graillat C, the Guyot A, Bourgeat-LamiE.Encapsulation such as Lelu
of an organic phthalocyanine blue pigment into polystyrene latex particles
using a miniemulsion polymerization process.Polym Int2003;52:542-7.] use thin breast
Liquid polymerization be prepared for polystyrene coated copper phthalocyanine dye nano-coloring material but, it is thus achieved that nano-coloring material particle morphology do not advise
Whole, reunite serious, particle diameter distribution width.
Liu Tao using aqueous polyurethane (isocynate-glycol polyurethane-WPU) as polymerisable emulsifier,
Mini-emulsion polymerization is used to prepare nano-coloring material [LiuT, LiZ, WuQ, MaX.Synthesis of nanocolorants with
crosslinked shell by miniemulsion polymerization stabilized by waterborne
polyurethane[J].PolymerBulletin,2009,64(5):511-21.].But the polyurethane price used is higher, very
Difficulty is applied in actual production.
Summary of the invention
It is an object of the invention to provide a kind of environment-friendly type nano coloring material aqueous dispersions and preparation method thereof, existing to overcome
Deficiency in technology.
Environment-friendly type nano coloring material aqueous dispersions of the present invention, it is characterised in that use alpha-olefin sodium sulfonate conduct
Polymerisable emulsifier, replaces conventional emulsifier, alpha-olefin sodium sulfonate energy and monomer copolymerization, and is therefore invariably present in dispersion body surface
Face, overcomes the problem that conventional emulsifier can ooze out from nano-coloring material, finally avoid nano-coloring material dispersion reunion precipitation
Defect.
Environment-friendly type nano coloring material aqueous dispersions described in the present invention, its component includes: water, alpha-olefin sodium sulfonate and other
The copolymer of monomer and dyestuff.
Dye distribution, in polymer, constitutes dispersion phase, and water is continuous phase；
The size of described dispersion phase is 80～100nm, particle diameter breadth coefficient 0.01～0.1；
Dispersion phase accounts for the 23.0%～38.0% of described aqueous dispersion weight；
Preferably, the percentage by weight of each component of aqueous dispersion is:
Copolymer 20.5%～33.8%
Dyestuff 1.3%～3.6%
Water 61.2%～76.5%；
Described dyestuff is made up of hydrophobic dye, co-stabilizer and light stabilizer；
The described copolymer that copolymer is alpha-olefin sodium sulfonate and other monomer.
Other described monomers refer to occur the monomer of Raolical polymerizable, are made up of principal monomer and cross-linking monomer；
Described principal monomer is selected from the monomer having bigger dissolubility to dyestuff, selected from styrene, vinyltoluene or uncle
Butylstyrene, acrylic acid, methacrylic acid, esters of acrylic acid, n-butyl acrylate, methyl methacrylate, metering system
Acid butyl ester, hydroxyethyl methylacrylate, acrylic acid lauryl alcohol ester；Optimization styrene, vinyltoluene, acrylic acid methyl ester. or methyl
Acrylic acid methyl ester.；
Described cross-linking monomer is selected from least two unconjugated olefines unsaturated double-bonds, or contains at least one alkene
Hydro carbons unsaturated double-bond and the polyfunctional monomer that another is carboxyl or hydroxyl, such as divinylbenzene, dimethacrylate
Glycol ester, allyl methyl acrylic acid, ethylene glycol diacrylate, butanediol diacrylate, dimethacrylate fourth two
Alcohol ester, neopentyl glycol dimethacrylate or dimethacrylate tetraethylene glycol (TEG)；Preferably divinylbenzene, dimethacrylate second
Diol ester, allyl methyl acrylic acid, ethylene glycol diacrylate；
Main monomer consumption accounts for the 90.9%～96.1wt% of monomer total amount, and the consumption of cross-linking monomer accounts for monomer total amount
3.8%～9.1wt%.
The consumption of described alpha-olefin sodium sulfonate accounts for the 0.9%～4.5wt% of copolymer quality.
The structural formula of described alpha-olefin sodium sulfonate is: CH3(CH2)nCH=CHCH2SO3Na
Wherein: n=14-16；
Described hydrophobic dye is dyes of anthraquinone, including redness, yellow, green or blue dyes, especially C.I.
Solvent red 168,146, C.I. solvent yellow 16 3,189, C.I. solvent green 3,28, C.I. solvent blue 36,45,97,3R；Preferably C.I.
Solvent blue 36, C.I. solvent yellow 189, C.I. solvent red 146.
Described co-stabilizer is selected from the alcohols of C12～C34, the alkane of C12～C24, octadecyl methacrylate, or ten
One or both mixture of dialkyl group mercaptan；Preferably octadecyl methacrylate, hexadecanol, lauryl mercaptan, 16
Alkane；The consumption of co-stabilizer is the 1.1%～3.6wt% of monomer total amount；
Described light stabilizer is steady selected from benzophenone light stabilizer, benzotriazole light stabilizer or hindered amines light
Determine agent, such as 2-hydroxyl-4 methoxy benzophenone, 2-(2 '-hydroxyl-3 ', 5 '-di-tert-butyl-phenyl)-5-chloro benzo three
Azoles, Tinuvin326, GW-540, GW-770, GW-622, GW-944, GW-628, GW-4611, preferably GW-540, GW-770,
GW-622、GW-944；Light stabilizer consumption is the 0.36%～0.96wt% of monomer total amount.
The preparation method of the environment-friendly type nano coloring material aqueous dispersions of the present invention, comprises the steps:
(1) alpha-olefin sodium sulfonate is dissolved in water, obtains alpha-olefin sodium sulfonate water solution A；
(2) dyestuff is joined in other monomer, mixed dissolution, obtain other monomer solution B containing dyestuff；
(3) preparation of other monomer miniemulsion containing dyestuff: at normal temperatures other monomer solution B containing dyestuff is joined
In water solution A, stir 15～25min, obtain thick emulsion, be subsequently placed in the environment of 0 DEG C～20 DEG C, use cutter to carry out all
Matterization processes, and obtaining the monomer miniemulsion C containing dyestuff, the preferably time of homogenizing is 10～60min；
(4) polymerization: by the monomer miniemulsion C containing dyestuff, under nitrogen protection, adds initiator, 40～90 DEG C, causes poly-
Closing, polymerization time is 2～12h, obtains the nano-coloring material aqueous dispersions of environment-friendly type.
Described initiator is radical initiator, mainly includes persulfuric acid salt initiator, azo-initiator or has
Machine peroxide initiator.Persulfuric acid salt initiator is selected from potassium peroxydisulfate, sodium peroxydisulfate, Ammonium persulfate. etc., and azo causes
Agent is selected from azodiisobutyronitrile (AIBN), AMBN, 2,2'-Azobis(2,4-dimethylvaleronitrile), azo-bis-iso-dimethyl etc., organic
Peroxide initiator can be benzoyl peroxide, cumyl peroxide etc.；Preferably potassium peroxydisulfate, azodiisobutyronitrile,
Dicumyl peroxide.
For water soluble starter, preferably the most before proceeding or adding in polymerization process, selecting excellent interpolation opportunity is to work as
After temperature reaches 40 DEG C, addition is the 0.24%～1.45wt% of monomer total amount, and being dissolved in water in advance before interpolation becomes
The aqueous solution of mass content 2%～10wt%, can disposably add, it is also possible to add for 2～3 times.
For oil-soluble initiator, preferably in the monomer solution preparation process containing dyestuff, add monomer solution to
In, addition is the 0.36%～3.6wt% of described monomer total amount.
Co-stabilizer, light stabilizer can add in the preparation process of other monomer solutions B containing dyestuff.
The effect of invention
The alpha-olefin sodium sulfonate that the environment-friendly type nano coloring material aqueous dispersions of the present invention uses be a kind of activity higher can
Polymerism or reactive emulsifier, the existing emulsifiability of this emulsifying agent, is again the monomer that a kind of activity is higher, can be single with other
Body is copolymerized.Other traditional reactive emulsifier, such as maleic anhydride list Palmitate carboxylic acid sodium etc., due to maleic acid unit
Polymerization activity the least, it is difficult to be copolymerized with the monomer such as acrylic compounds and styrene, especially there is bigger ester group
After unit, its polymerization activity is less, and therefore, for the storage stability of nano-coloring material aqueous dispersions, Malaysia acids is anti-
Answer type emulsifying agent not significant advantage compared with nano-coloring material prepared by non-reactive emulsifying agent.
In the course of the polymerization process, dyestuff and polymer occur to be separated and form gathering and be embedded into macromole net mutually the present invention
The inside of network, the crosslinking of polymer then can significantly stop the motion of dye aggregation phase to migrate, thus improve the resistance to of colorant and move
Shifting property and colour brightness.Polymerization monomer adds appropriate light stabilizer so that after polymerization, nano-coloring material particle is structurally
There is the performance that light is stable, the light stability of colorant can be greatly improved.It is different from the physics such as mechanical lapping, comminution by gas stream
The ultra-fine colorant that method prepares, by hydrophobic dye is dissolved in certain monomer during the nano-coloring material that the present invention provides
The inside, after polymerization, prepares the coloured polymer aqueous dispersion of nano-scale, and the most this nano-coloring material is at water
There is in mutually excellent storage stability.
Detailed description of the invention
The test instrunment that the present invention uses is as follows: with ultraviolet-visible spectrometer (Prism Optical Technology Co S53/54
Type) measure the absorbance of nano-coloring material, use Photon Correlation Spectrum instrument (Zetasizer Nano S, Malvern Instruments)
Measure mean diameter and the particle diameter distribution of nano-coloring material.Particle diameter breadth coefficient uses the laser particle size that Malvern company of Britain produces
Instrument measures.
Dyestuff is the investigation method of resistance to migration in nano-coloring material: by color obtained after nano-coloring material latex lyophilization
Powder is dissolved in oxolane, then it is carried out uv-visible absorption spectra relative analysis, if the nano-coloring material just prepared is 0
The maximum absorbance that moment records is A0, the absorbance of t is At, then the relative surplus absorbance of t is defined as: relatively
Residue absorbance=At/A0× 100%, sample is placed 90 days, if its relative surplus absorbance is not less than 95%, is then evaluated as excellent
Elegant.
The storage stability of nano-coloring material aqueous dispersions investigates method: sample is put 120 days at room temperature, sees whether out
Now flocculate, precipitation etc., if without flocculation or precipitate after 120 days, being then evaluated as outstanding.
Embodiment 1
Take 2.0g alpha-olefin sodium sulfonate to be dissolved in 100g deionized water, be denoted as A1 component, standby；By 40g styrene,
1.6g divinylbenzene, 2.0gC.I. solvent blue 36,0.6g hexadecane, 0.4g light stabilizer GW-544 mix homogeneously, it is denoted as B1
Component.Component B1 is added drop-wise to in the 250mL beaker of churned mechanically Sheng component A of 200r/min；After 20min, by this breast
Liquid is put into and is used high-shear homogenizer micronization processes in ice-water bath, and rotating speed is 15000r/min, obtains miniemulsion after refinement 60min.
The miniemulsion prepared is transferred in the flask equipped with agitator, thermometer, condenser and nitrogen tube, blasts
30min nitrogen removes oxygen, then heats to 40 DEG C, then dropping 0.1g water soluble starter potassium peroxydisulfate is molten under nitrogen protection
Solution aqueous solution in 5g deionized water, starts to cause polymerization.After 70 DEG C of reaction 3h, through filtration treatment, by a small amount of gel
And aggregate impurity removes, obtain environment-friendly type nano coloring material aqueous dispersions.
After reaction terminates, obtain blue nano-coloring material aqueous dispersions.Wherein solid content is 37.2%(wt).At room temperature
After placing 4 months, there is no Precipitation, narrow diameter distribution, there is excellent storage stability and resistance to migration.The colorant of preparation
The performance of aqueous dispersion is shown in Table 1.
The chemical name of light stabilizer GW-544 is tris phosphite (TEMPO), can
Use the product of Beijing addition auxiliary agent research.
Embodiment 2
Take 0.5g alpha-olefin sodium sulfonate to be dissolved in 100g deionized water, be denoted as A2 component, standby；By 50.0g vinyl
Toluene, 5.0g Ethylene glycol dimethacrylate, 2.0g azodiisobutyronitrile, 6.0gC.I. solvent yellow 189,0.6g hexadecanol,
0.2g light stabilizer hindered amine 770 mix homogeneously, is denoted as B2 component.Component B2 be added drop-wise to 200r/min is churned mechanically
Contain in the 250mL beaker of component A2；After 20min, this emulsion being put into and use high-shear homogenizer micronization processes in ice-water bath, rotating speed is
20000r/min, obtains miniemulsion after refinement 10min.
The miniemulsion prepared is transferred in the flask equipped with agitator, thermometer, condenser and nitrogen tube, blasts
30min nitrogen removes oxygen, then heats to 40 DEG C, starts to cause polymerization.After 90 DEG C of reaction 10h, through filtration treatment, will be few
The gel of amount and aggregate impurity remove, and obtain environment-friendly type nano coloring material aqueous dispersions.
After reaction terminates, obtain Yellow nanometer coloring material aqueous dispersions.Wherein solid content is 40.0%(wt).At room temperature
After placing 4 months, there is no Precipitation, narrow diameter distribution, there is excellent storage stability and resistance to migration.The colorant of preparation
The performance of aqueous dispersion is shown in Table 1.
The chemical name of light stabilizer hindered amine 770 is double (2,2,6,6-tetramethyl-4-piperidyl) SA esters.Can adopt
GW-480 product with Beijing addition auxiliary agent institute.
Embodiment 3
Take 0.5g alpha-olefin sodium sulfonate to be dissolved in 100g deionized water, be denoted as A3 component, standby；By 30g metering system
Acid methyl ester, 2.5g allyl methyl acrylic acid, 2.5gC.I. solvent red 146,0.8g lauryl mercaptan, 0.2g light stabilizer
GW-622 mix homogeneously, is denoted as B3 component.Component B3 is added drop-wise to the 250mL of churned mechanically Sheng component A3 with 100 revs/min
In beaker；After 20min, this emulsion being put into and use high-shear homogenizer micronization processes in ice-water bath, rotating speed is 15000r/min, refinement
Miniemulsion is obtained after 20min.
The miniemulsion prepared is transferred in the flask equipped with agitator, thermometer, condenser and nitrogen tube, blasts
30min nitrogen removes oxygen, then heats to 65 DEG C, then addition 0.5g potassium peroxydisulfate is dissolved in 5g deionization under nitrogen protection
Solution in water, starts to cause polymerization.After 65 DEG C of reaction 5h, through filtration treatment, a small amount of gel and aggregate impurity are removed
Go, obtain environment-friendly type nano coloring material aqueous dispersions.
After reaction terminates, obtain Yellow nanometer coloring material aqueous dispersions.Wherein solid content is 25.3%(wt).At room temperature
After placing 4 months, there is no Precipitation, narrow diameter distribution, there is excellent storage stability and resistance to migration.The colorant of preparation
The performance of aqueous dispersion is shown in Table 1.
The chemical name of light stabilizer GW-622 is poly-(1-ethoxy-2,2,6,6-tetramethyl-4-hydroxy piperidine) fourth two
Acid esters, can use GW-622 or the Ciba-Geigy company's T inuvin622LD product of Beijing addition auxiliary agent institute.
Embodiment 4
Take 1.0g alpha-olefin sodium sulfonate to be dissolved in 100g deionized water, be denoted as A4 component, standby；By 25g acrylic acid first
Ester, 2.5g ethylene glycol diacrylate, 0.1g dicumyl peroxide, 2.5gC.I. solvent red 146,1.0g methacrylic acid 18
Ester, 0.2g light stabilizer GW-944 mix homogeneously, be denoted as B4 component.Component B4 is added drop-wise to the mechanical agitation of 1500 revs/min
Sheng component A4 250mL beaker in；After 20min, this emulsion is put into ice-water bath is used high-shear homogenizer micronization processes, rotating speed
For 18000r/min, after refinement 20min, obtain miniemulsion.
The miniemulsion prepared is transferred in the flask equipped with agitator, thermometer, condenser and nitrogen tube, blasts
30min nitrogen removes oxygen, then heats to 75 DEG C, then addition 0.4g potassium peroxydisulfate is dissolved in 5g deionization under nitrogen protection
Solution in water starts to cause polymerization.After 75 DEG C of reaction 6h, through filtration treatment, a small amount of gel and aggregate impurity are removed
Go, obtain environment-friendly type nano coloring material aqueous dispersions.
After reaction terminates, obtain Yellow nanometer coloring material aqueous dispersions.Wherein solid content is 22.7%(wt).At room temperature
After placing 4 months, there is no Precipitation, narrow diameter distribution, there is excellent storage stability and resistance to migration.The colorant of preparation
The performance of aqueous dispersion is shown in Table 1.
The chemical name of light stabilizer GW-944 be poly-([6-[1,1,3,3-tetramethyl butyl)-imino group]-1,3,5-
Triazine-2,4-diyl] [2-(2,2,6,6-tetramethyl-piperidyl)-secondary amino-hexa-methylene-[4-(2,2,6,6 ,-tetramethyl piperazine
Piperidinyl)-secondary amino], GW-944z or the Ciba company limited of Switzerland of Beijing addition auxiliary agent institute can be used
The product of CHIMASSORB944FD.
Comparative example 1
Take 2.0g dodecylbenzene sodium sulfonate to be dissolved in 100g deionized water, be denoted as component A, standby；By 40g benzene second
Alkene, 1.6g divinylbenzene, 2.0gC.I. solvent blue 36,0.6g hexadecane, 0.4g light stabilizer GW-544 mix homogeneously, it is denoted as
B component.Component B is added drop-wise to in the 250mL beaker of churned mechanically Sheng component A of 200 revs/min；After 20 minutes, by this breast
Liquid is put into and is used high-shear homogenizer micronization processes in ice-water bath, and rotating speed is 15000 revs/min, obtains miniemulsion after refining 60 minutes.
The miniemulsion prepared is transferred in the flask equipped with agitator, thermometer, condenser and nitrogen tube, blasts
30min nitrogen removes oxygen, then heats to 40 DEG C, then dropping 0.2g water soluble starter potassium peroxydisulfate is molten under nitrogen protection
Solution aqueous solution in 5g deionized water, starts to cause polymerization.After 70 DEG C of reaction 3h, through filtration treatment, by a small amount of gel
And aggregate impurity removes, obtain environment-friendly type nano coloring material aqueous dispersions.
After reaction terminates, obtain blue nano-coloring material aqueous dispersions.Wherein solid content is 38.6%(wt).At room temperature
After placing 4 months, having a small amount of Precipitation, particle diameter distribution width, storage stability and resistance to migration are the best.That prepares is coloring material aqueous
The performance of dispersion is shown in Table 1.
The chemical name of light stabilizer GW-544 is tris phosphite (TEMPO), can
Use the product of Beijing addition auxiliary agent research.
Table 1: the performance of nano-coloring material aqueous dispersions prepared by embodiment 1～4 and comparative example
Claims (7)
1. environment-friendly type nano coloring material aqueous dispersions, it is characterised in that its component includes: water, alpha-olefin sodium sulfonate are single with other
The copolymer of body and dyestuff, dye distribution, in polymer, constitutes dispersion phase, and water is continuous phase；The size of described dispersion phase is
80～100nm, particle diameter breadth coefficient 0.01～0.1；Dispersion phase accounts for the 23.0%～38.0% of described aqueous dispersion weight, respectively
The percentage by weight of individual component is:
Copolymer 20.5%～33.8%
Dyestuff 1.3%～3.6%
Water 61.2%～76.5%；
Described dyestuff is made up of hydrophobic dye, co-stabilizer and light stabilizer, described copolymer be alpha-olefin sodium sulfonate with
The copolymer of other monomer, other described monomers are made up of principal monomer and cross-linking monomer；
Described principal monomer is selected from styrene, vinyltoluene or t-butyl styrene, acrylic acid, methacrylic acid, propylene
Acid N-butyl, methyl methacrylate, butyl methacrylate, hydroxyethyl methylacrylate, acrylic acid lauryl alcohol ester；
Described cross-linking monomer is selected from divinylbenzene, Ethylene glycol dimethacrylate, allyl methyl acrylic acid, two propylene
Acid glycol ester, butanediol diacrylate, tetramethylene dimethacrylate, neopentyl glycol dimethacrylate or diformazan
Base acrylic acid tetraethylene glycol (TEG).
Environment-friendly type nano coloring material aqueous dispersions the most according to claim 1, it is characterised in that principal monomer consumption accounts for list
The 90.9%～96.1wt% of body total amount, the consumption of cross-linking monomer accounts for the 3.8%～9.1wt% of monomer total amount.
Environment-friendly type nano coloring material aqueous dispersions the most according to claim 1, it is characterised in that described alpha-olefin sulfonic acid
The consumption of sodium accounts for the 0.9%～4.5wt% of copolymer quality.
4. according to the environment-friendly type nano coloring material aqueous dispersions described in any one of claim 2～3, it is characterised in that described
The structural formula of alpha-olefin sodium sulfonate is: CH3(CH2)nCH=CHCH2SO3Na, wherein: n=14-16.
Environment-friendly type nano coloring material aqueous dispersions the most according to claim 1, it is characterised in that described hydrophobic dye
Dyes of anthraquinone, including redness, yellow, green or blue dyes, described co-stabilizer selected from octadecyl methacrylate,
Hexadecanol, lauryl mercaptan, hexadecane；The consumption of co-stabilizer is the 1.1%～3.6wt% of monomer total amount；Described light
Stabilizer is selected from GW-540, GW-770, GW-622, GW-944；Light stabilizer consumption be monomer total amount 0.36%～
0.96wt%.
6., according to the preparation method of the environment-friendly type nano coloring material aqueous dispersions described in any one of claim 2～5, its feature exists
In, comprise the steps:
(1) alpha-olefin sodium sulfonate is dissolved in water, obtains alpha-olefin sodium sulfonate water solution A；
(2) dyestuff is joined in other monomer, mixed dissolution, obtain other monomer solution B containing dyestuff；
(3) preparation of other monomer miniemulsion containing dyestuff: at normal temperatures other monomer solution B containing dyestuff is joined water-soluble
In liquid A, stir 15～25min, obtain thick emulsion, be subsequently placed in the environment of 0 DEG C～20 DEG C, use cutter to homogenize
Processing, obtaining the monomer miniemulsion C containing dyestuff, the preferably time of homogenizing is 10～60min；
(4) polymerization: by the monomer miniemulsion C containing dyestuff, under nitrogen protection, adds initiator, 40～90 DEG C, causes polymerization,
Polymerization time is 2～12h, obtains the nano-coloring material aqueous dispersions of described environment-friendly type；
Described initiator is persulfuric acid salt initiator, azo-initiator or organic peroxide evocating agent.
Method the most according to claim 6, it is characterised in that for water soluble starter, before proceeding or be polymerized
Adding in journey, addition is the 0.24%～1.45wt% of monomer total amount, and being dissolved in water in advance before interpolation becomes quality and contain
The aqueous solution of amount 2%～10wt%, disposable interpolation or point 2～3 interpolations；
For oil-soluble initiator, adding in monomer solution in the monomer solution preparation process containing dyestuff, addition is
The 0.36%～3.6wt% of described monomer total amount；
Co-stabilizer, light stabilizer add in the preparation process of other monomer solutions B containing dyestuff.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| EP0796876A1 (en) * | 1996-03-22 | 1997-09-24 | National Starch and Chemical Investment Holding Corporation | Dye compositions and methods for the manufacture thereof |
| CN100497489C (en) * | 2006-11-23 | 2009-06-10 | 上海交通大学 | Method for preparing nano pigment water-borne dispersion |
| CN101362865A (en) * | 2007-08-10 | 2009-02-11 | 深圳市海川实业股份有限公司 | Method for preparing nano colouring matter aqueous dispersions |
| CN101486845A (en) * | 2008-01-14 | 2009-07-22 | 深圳市海川实业股份有限公司 | Method for preparing nano colouring matter aqueous dispersions |
| CN101220230A (en) * | 2008-01-30 | 2008-07-16 | 上海华明高技术（集团）有限公司 | Nano-coloring material aqueous dispersions containing polyurethane component and method for producing the same |
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