CN1299830C - Super-micro particle dispersing and milling method and product - Google Patents

Abstract

The present invention relates to a supermicro particle dispersing and grinding method which mainly comprises the steps that a substrate, a dispersing agent and dispersion media are firstly mixed into a mixture, secondly a pre-processed grinding medium is orderly provided, the grinding medium is added in the mixture, the grinding medium is glass balls with the average grain diameter smaller than 100 mu m, the mixture is ground, and finally the grinding medium is separated from dispersion liquid. The present invention also relates to pigment paste prepared by the dispersing and grinding method.

Description

Ultramicron dispersing and milling method and goods thereof

Technical field

The invention relates to a kind of Ginding process, refer in particular to a kind of ultramicron dispersing and milling method.The invention still further relates to the goods color of above-mentioned ultramicron dispersing and milling method.

Background technology

General nanometer (nm) grade particle disperses employed super-fine-ground medium that two classes are arranged, and one is the higher metal carbides of material hardness, and another is the lower macromolecule material abrasive media of hardness.When using the higher abrasive media of hardness to disperse, for example use the fine abrasive media of higher yttrium zirconium of density or metal carbides material, the thing to be disperseed that then often causes institute's desire to be disperseed is polluted by the material that grinds cell wall, abrasive media hardness is too high to cause grinding groove wearing and tearing, dispersion liquid product colour deviation, heavy metal or chemical analysis to pollute or the potential of hydrogen scope set etc. that surpasss the expectation in order to avoid, usually must select the grinding groove and the dispersive element of hard relatively material for use, but such equipment material costliness will make that equipment cost greatly improves.

And if use the macromolecule abrasive media, then can make the material ranges of grinding groove or blade will be more extensively and comparatively cheap, but because of macromolecule hardness lower, the powder that therefore can disperse only can be confined on the organic powder soft and easily dispersion or depolymerization, and cause colliding because of its density is low strength little, have floating phenomenon and take place, and dispersion efficiency is poor.In addition, its surface free energy is lower and the bubble compatibility is big, easily has bubble to produce, and this can make grinding system become bubble/abrasive media/three kinds of constituents of dispersed paste, occur local static, can't stir the state of mixing.That is (＜30nm) branch lively stock (US), because the density of the abrasive media of its use is lower, dispersion efficiency is relatively poor to use the fine abrasive media of polymer electrolyte to carry out nano-scale.

Summary of the invention

Main purpose of the present invention is that a kind of ultramicron dispersing and milling method is being provided, so that can reduce equipment cost, avoids abrasive media to pollute and wearing and tearing, and reaches the effect of high efficiency particle miniaturization.

Another object of the present invention is that a kind of ultramicron dispersing and milling method is being provided, so that can make the pigment powder reach the dispersion effect of nanoscale (less than 30nm), to improve its color degree of saturation and color developing.

Another object of the present invention is that a kind of color is being provided, and is the goods that utilize above-mentioned ultramicron dispersing and milling method to make, and is to utilize high miniaturization pigment particles evenly to disperse, and improves the saturation degree of color.

For reaching above-mentioned purpose, a kind of ultramicron dispersing and milling method provided by the invention mainly may further comprise the steps:

(a) matrix, dispersant are mixed with the dispersion medium a mixture;

(b) provide once pretreated abrasive media, and this abrasive media is added in this mixture; Wherein this abrasive media is the glass marble of average grain diameter less than 100 μ m;

(c) grind this mixture; And

(d) this abrasive media is separated in this dispersion liquid.

Described ultramicron dispersing and milling method, wherein this matrix is embarrassed soluble dye, pigment, is had crystalline organic matter, macromolecule or medicament powder.

Described ultramicron dispersing and milling method, wherein this dispersant is to be selected from a group that is made up of anionic, cationic, nonionic and polymer electrolyte interfacial agent and composition thereof.

Described ultramicron dispersing and milling method, wherein this dispersion medium is to be selected from a group that is made up of water, saline solution, methyl alcohol, ethanol, butanols, hexane, ethylene glycol and composition thereof.

Described ultramicron dispersing and milling method should be to screen in water overflow mode through pretreated abrasive media wherein.

Described ultramicron dispersing and milling method, wherein the average grain diameter of this abrasive media is between 50 to 100 μ m.

Described ultramicron dispersing and milling method, wherein the density of this abrasive media is to 3g/cm between 1 ³Between.

Described ultramicron dispersing and milling method, wherein to grind this mixture be to be ground to the average grain diameter of this matrix less than 100nm to step (C).

Described ultramicron dispersing and milling method, wherein this abrasive media is a spherical shape.

Described ultramicron dispersing and milling method, wherein grinding is to finish with a grinder, this grinder also comprises a stainless steel mixing channel and a stirring vane.

Described ultramicron dispersing and milling method, wherein this grinder is a kind of in air type grinder (airiermill), roller grinder (roller mill), ball mill (ball mill), mixer grinder (attritormill), vibration-type grinder (vibratory mill), planetary-type grinding machine (planetary mill), sand milling (sand mill) machine or the ball mill (bead mill).

Described ultramicron dispersing and milling method, its operation pattern is batch, continous way or half batch.

Described ultramicron dispersing and milling method, its be used to make color with pigment, coating with pigment, polymer with pigment or pigment for printing ink.

For achieving the above object, a kind of color that utilizes above-mentioned ultramicron dispersing and milling method to make provided by the invention is mainly to comprise:

0.1 to the pigment of 70 weight portions, wherein the average grain diameter of this pigment is less than 100nm;

0.1 dispersant to 30 weight portions; And

The water of 40 to 90 weight portions;

Wherein this pigment is with dispersant and disperses medium to mix; Through average grain diameter be ground to less than the glass marble of 100 μ m average grain diameter less than 100nm after; In this dispersion liquid, separate and get.

Described color, wherein this dispersant is to be selected from a group that is made up of anionic, cationic, nonionic and polymer electrolyte interfacial agent and composition thereof.

The invention has the advantages that,, avoid abrasive media to pollute and wearing and tearing, and reach the effect of high efficiency particle miniaturization, improve the saturation degree of color color so that can reduce equipment cost.

Description of drawings

Fig. 1 be the embodiment of the invention 3 pigment disperse particle diameter through the time result of variations.

The specific embodiment

Ultramicron dispersing and milling method of the present invention is mainly utilized the glass grinding media less than 100 microns, in the wet lapping mode, powder with the desire dispersion, help the dispersant that disperses, and after providing the dispersion medium that disperses powder and dispersant to be mixed into a mixture, add abrasive media again in aforementioned mixture, again with a Mixing Machine device, as grinder, provide one to drive energy, make abrasive media produce collision strength, and drive said mixture, make to produce between its fluid and solid or solid and solid and shear strength and collision strength, thereby make the dispersion powder body micronizing that is present between abrasive media.Grinder comprises the element of a drive abrasive media or the energy of its motion is provided, and a splendid attire should be desired the container of dispersed mixture and abrasive media.Below disperse powder kind and dispersion pattern etc. to describe at abrasive media of the present invention, dispersion, dispersion medium, dispersant kind, desire.

The abrasive media material is inorganic glass material, and density is 1～3g/cm ³, spherical shape, irregularly shaped component content is low, if too high levels then needs with removal, as removing in modes such as gravity, filtration, screen analysises and separating.In addition, this abrasive media also can and bigger with particle, single the abrasive media that density is lower, and the different abrasive media that has equivalent weight with abrasive media that the present invention uses, the abrasive media of this and usefulness is the polymer electrolyte abrasive media mostly, they can be crosslinked polystyrene (cross linked polystyrenes), polystyrene copolymer (styrene copolymers), Merlon (polycarbonates), poly-inferior aldehyde (polyacetals), polyvinyl chloride (vinylchloride polymers) and polyvinyl chloride copolymer (polyurethanes) thereof, polyamine polyamides), band fluoropolymer polymer (fluoropolymers), high density polyethylene (HDPE) (highdensity polyethylenes), polypropylene (polypropylenes)), cellulose ether-esters cellulose ethers and esters), acryl polymer (polyacrylates) and contain silicon polymer (silicone cantaining polymers) etc.

The size of abrasive media has 1/1000 empirical relation approximately with the final fineness ratio of dividing lively stock.Abrasive media is 100 microns fineness of dispersion products that can disperse acquisition＜100nm.Abrasive media is 50 microns, can obtain the fineness of dispersion product less than 50nm.The abrasive media particle diameter is healed the fineness of little products obtained therefrom will be littler.But the initial dispersion size of the powder that desire is disperseed can not be excessive, and is unsuitable near the person with the abrasive media size.If soft aggregation, dispersible suitable size is less than 1/3 of abrasive media size, is preferably less than 1/10 of abrasive media.If hard or be the inorganic particle material, then abrasive media must be comparatively suitable greater than ten times of this kind powder aggregation size.

Grinding dispersion can be that dry type (as dry roller mill) or wet type are disperseed (wet-milling), preferably uses the wet type dispersing mode to carry out.Be used as the liquid that disperses media, be called the dispersion medium, i.e. liquid composition, it mainly provides dispersant (interfacial agent or dispersing aid) and disperses powder to have the media liquid in space.They can be water, saline solution, methyl alcohol, ethanol, butanols, hexane, ethylene glycol and other organic solvent or its mixture etc.And dispersant can be selected from listed material in the special book of general interface activating agent, and its addition is about and disperses 0.1～90% of powder composition weight.

The kind that dispersant uses is relevant with the chemical constitution and the characteristic of the powder that desire is disperseed.It structurally has the characteristic of surface absorption usually, the powder surface that one end disperses for desire has good compatibility, the other end is then to disperseing medium to have good matchmaker to close characteristic, and can effectively stretch, produce steric hindrance, or have electronegative or electropositivity produces the electrostatic repulsion effect at this close matchmaker end, make that the powder particle that has disperseed no longer contacts, gathering and steady.Usually the group of the close powder of dispersant preferably with the chemical constitution or the close person of physical characteristic of powder, affine, the adsorption effect that just has like this, they are generally the group of long carbochain or have full closing or cyclic compound that insatiable hunger is closed, separately the compound or derivatives thereof of structure genetic system etc.Close matchmaker's base is then looked the characteristic of disperseing medium and different, if the dispersion medium that polarity is higher, then select the material that is used as this group with the higher group of polarity for use as water or aqueous solution, have the electrical ionic group of yin, yang and can produce the structure of hydrogen bonds group, as SO ₃Na, COONa, (CH ₂CH ₂O) n, SO ₄Na, OH.All types of interfacial agents such as the anionic in special book of general interface activating agent and paper, mentioned; Cationic and the nonionic or the interfacial agent of polymer electrolyte; Or the mixture of any combination of the interfacial agent of aforementioned four kinds of patterns meets, and aforementioned dispersion important document person all is suitable for; Be preferably polyacrylic acid (Polyacrylate); Sulfonated aromatic base aldehyde condensate (Formaldehyde condensates of sulfonatedaromatic compounds); Light base of polyethoxy or aryl (Conventional alkyl oralkryl polyethoxylates); Polyamine base formaldehyde (Polyurethane type); Core-shell type polymer (Core-shell Polymer); Polyester (Polyester); Polyaminoacid (Polyaminoacid dispersant); Agglomerate copolymer (Block copolymer); Photo-crosslinking type polymer (Photo-crosslinkable polymeric dispersant); Star polymer (Starpolymer); Polyamine/polyglycerol fatty acid condensation product (Polyamine/fatty acid condensationpolymeric dispersant); Upgrading polypropylene amine (Modified acrylamide oligomerdispersant); Be more preferred from Ju Yangization Yi Xi Ring ether tetrahydrochysene alcohol fatty acid ester (Polyoxyethylenesorbitan fatty acid ester); Hot phenyl polyethylene glyceride (Octyl (phenolpolyethylene glycol ether); Poly alkyl alcohol Ethylene Glycol ester (Fatty alcoholpolyethylene glycol ether); Polypropylene polyethylene glycol oxide ester (Polyoxypropylenepolyoxyethylene ether); Fatty acid polyethylene glyceride (Fatty acidpolyethylene glycol ether); Castor oil polyethylene glyceride (Castor oilpolyethylene glycol ether); Sulfosuccinic Single ethene (Sulfosuccinatemonoester); Two octyl group butanedioic acids (di-octyl sulfouccinate); Dodecyl benzene sulfonic acid (dodecyl benzene sulfonate); The two alkyl Jia Liu Suan ization things (miscellaneousdialkyl ammonium methosulfate) of naphthaldehyde condensation compound (naphthaleneformal dehyde condesate) Wei Zhi Body; Polyethylene glycol oxide Arrcostab (polyoxethylenealkyl ether); Polyethylene glycerine fatty acid (polythylene glycol fatty acid, ethyoxyl amide (amine ethoxylate); Polyethylene glycol oxide double styrene phenol (polyoxylethylene di-styrenated phenol); Nonyl phenylester phosphorylation thing (Nonyl phenyl ether phosphate); Polyethylene glycol oxide double styrene cresols (Polyoxyethylene di-styrenated cresol) Shrink closes aromatic hydrocarbon sulfonic acid (Condensated arylsulfonic acid); The aromatic polyester substrate disperses Elixirs (Aromaticpolyether based dispersant); Benzene alkane ethyoxyl (Alkylphenol ehtoxylates) With butyl glycerine (butyl glycol); Right-methyl-Right-oily anilide taurine thing (N-methyl-N-oleoyl taurate).

Utilizing the present invention the micronize of incombustible agent, medicament powder and the crystallinity function powder etc. of the pigment of disperse dyes, fluorescent whitening dyestuff, coating and printing ink, organic or inorganic can be ground disperses; the particle that can obtain time micron and nano-scale divides lively stock; be particle diameter less than 500nm, disperse preferably to reach particle diameter less than 100nm or particle diameter less than 30nm.Utilize decentralized system of the present invention that situations such as serious abrasive media pollution and abrasive media wearing and tearing can't take place, products obtained therefrom does not have the generations such as problem of the serious deviation of color yet.

Grind the processing procedure that disperses and to use different types of grinder.Suitable grinder can comprise air type grinder, roller grinder, ball mill, mixer grinder, vibration-type grinder, planetary-type grinding machine, sand mill or ball mill.Device with the dispersion of high-energy abrasive media is preferable selection, can have an axle center of rotating.The operation that grind to disperse can be batch, continous way or half batch pattern, is described as follows.

Batch grind to disperse use the mixing arrangement of motor and stirring vane, with particle diameter less than 100 microns glass grinding media, disperse medium, desire to disperse powder particle, dispersant.The milling apparatus that afterwards this mixture is placed traditional high-energy batch polish process to use.As high speed skiving dispersion machine, vibration-type grinder, ball mill etc.This mixed slurry will disperse with certain hour, so that desire disperses the powder particle particle diameter to drop to the dispersion size of expectation.After disperseing to finish, will divide lively stock (powder particle that has disperseed, dispersant and disperse medium) to filter with abrasive media or sieve from.

Continous way grind to disperse uses particle diameter less than 100 microns glass grinding media, it disperses the mixture of powder particle and dispersant to be cycled through continuously in the traditional abrasive media dispersion machine (media mill) by an external mix groove with disperseing medium, desire, this dispersion machine has a medium separate mesh or a gap, can adjust the dispersed mixture that makes less than 100 microns and freely pass through in the pipeline of circulation.After five equilibrium clears, will divide lively stock (powder particle that has disperseed, dispersant and disperse medium) to filter with abrasive media or sieve from.The mixed grinding medium milling disperses, disperse powder particle and mixture of dispersing agents to cycle through continuously in the traditional abrasive media dispersion machine that contains greater than 250 microns abrasive medias less than 100 microns glass grinding media, dispersion medium, desire particle diameter by an external mix groove, this dispersion machine has a medium separate mesh or a gap, big abrasive media is stayed in grind in the cell body, and make less than in 100 microns the abrasive media and the pipeline of dispersion product mixture freedom by the grinding groove circulation.After five equilibrium clears, will divide lively stock (powder particle that has disperseed, dispersant and disperse medium) to filter with abrasive media or sieve from, can use traditional filtering technique to separate, as filter, screen analysis crosses a fixed network purpose mesh screen or akin method.

Milling time has great difference with disperseing powder kind, initial size and final fineness, dispersal device and scatter operation pattern.Can the holdup time of dispersed mixture in grinding system index as a comparison.The general ball mill time long by a couple of days to several weeks, traditional abrasive media dispersion machine then needs about eight hours operating time.

Your for allowing juror can more understand technology contents of the present invention, be described as follows especially exemplified by the preferred embodiment of ultramicron dispersing and milling method.

The preliminary treatment of embodiment 1 abrasive media

(A) original abrasive media impurity separates: get l00g precision glass ball (PrecisionGlass Spheres, Class V), particle size range 53-45 μ m (MO-SCI SpecialtyProducts, L.L.C.) abrasive media, be placed on a long tubular, the bottom has after filtration, and the water of 5 microns filters flows into, the top has in the glassware of spout hole, the water flux density that flows into these vessel is adjusted to the glass grinding media that is present in the container has stable suspension, and the upper strata power that has the weight of a little particulate to overcome up to flow and overflow and go out.Continue to make current to pass to till the abrasive media particle exists hardly.Original abrasive media (sample 1-1), the abrasive media that overflows are collected (sample 1-2) and are collected detection with the abrasive media (sample 1-3) that does not overflow.

(B) carry out separating impurity after the high-speed stirred without separation: with 100g water mix with the volume be the abrasive media of 100ml with the 40mm blade, rotating speed 5000rpm stirs collision, continues to carry out to stop after 10 hours.This mixed liquor is inserted employed separator in (A), separate in the same manner, collect the abrasive media (sample 1-4) that overflows.

Presentation of results: the sample that abovementioned steps is collected, observe with light microscope, show in the original abrasive media (sample 1-1) and contain different impurities, as irregular, black person and particle diameter smaller.Irregularly shaped have a sharp-pointed water caltrop, can stress after the dispersion concentrated and cracked.Include bubble in the black person, under illumination,, can show black because of the relation of refraction, may be cracked under the grinding high velocity impact.Particle diameter is less then easily to be the big slightly person's wearing and tearing of other particle diameter.These compositions all must be removed before grinding dispersion.And the abrasive media that overflows (sample 1-2) demonstration is particle diameter smaller, black person and irregularly shaped person.The abrasive media that does not overflow (sample 1-3) shows that abrasive media is very even after treatment, and impure composition is all removed.And with after step (B) high-speed stirred, isolate by levigate irregular composition (sample 1-4) through overflow.Know abrasive media if the unprocessed impure composition (irregularly shaped, black person, and particle diameter smaller) of isolating by aforementioned test, when grind stirring, can produce tiny a little cracked because of high velocity impact, or the surface of the abrasive media of these cracked meeting scratch normal conditions, the dispersion liquid product that desire is ground is polluted.Therefore, such separating step is essential, all must consider such processing pattern for the abrasive media of unlike material, otherwise the dispersion liquid product will be subjected to the pollution of the impure composition of abrasive media or its sliver.

The test of the suitable property of embodiment 2 abrasive medias and grinding groove

With 100g, density is 6g/cm ³, particle diameter is 38～75 microns yttrium zirconium material abrasive media, mixes with the water with volume, with the stainless steel blade of 40mm, rotating speed 5000rpm stirs collision, continues to carry out to stop after 10 hours.

The result: with perusal, after this experiment was carried out about two hours, the aqueous solution of stirring promptly began have black to manifest, and the time, longer color was darker.Because of the color of this kind abrasive media is a rice white, so the source of this color can determine not to be that the attrition of self-grind medium is cracked.Moreover the grinding groove that uses is stainless steel, and its hardness is low than abrasive media, therefore, can confirm that this change in color mainly is to be produced by the abrasive media wearing and tearing from the grinding groove surface.Carry out the test result demonstration of 50 microns beades with identical condition, the grinding groove wearing and tearing are not arranged and cause the situation of variable color to take place.Though the particle diameter of hence one can see that abrasive media drops to＜100 microns, the quality of its single medium and impact force be with less, uses the bigger yttrium zirconium material abrasive media of the density stainless steel tank that still can wear and tear.Therefore, fine abrasive media that this kind density is higher and the grinding that is not suitable for lower-cost stainless steel tank are used, and it is comparatively suitable to change with the abrasive media of glass material.

Embodiment 3 grindings of the present invention disperse processing procedure

Its minute, powder formula was listed in the table below 1.At first water and dispersant are inserted in the 1L grinding groove, diameter 40mm～50mm zigzag blade (colwes-type) and mixer (ULTRA-TURRAXT50basic is equipped with in use, IKA), dissolve with the 300rpm stirring at low speed, afterwards pigment is slowly added in the aqueous dispersant, waited to add the back stir about 1 hour.Abrasive media is slowly added in the dispersion liquid of aforementioned preparation, treat its fully moistening after, motor rotary speed slowly is increased to stirring vane speed, and (rotating speed is about 5000～8000rpm) under the state of 15m/s, continue to grind dispersion, in the process took a sample in every interval in about 1 hour, make particle size measuring to know the change of size of dispersion process with Malvern 4700, the pigment of result such as Fig. 1 present embodiment disperses particle diameter result over time, show and use glass grinding media to have the effect of efficient dispersion at about dispersion effect that promptly had less than 30nm in about six hours.Disperse to reach (being that particle diameter is less than 30nm) behind the predeterminated target specification particle diameter, it is 10% that the gauge water of dispersion liquid adding soon is diluted to about pigment weight content, use the filtering head little to separate with abrasive media afterwards, simultaneously the filter material of dispersion liquid with 1 micron hole size filtered isolated dispersion liquid with the dispersion liquid of suction device with the nano-scale size than abrasive media.

1 250 microns polystyrene materials of comparative example abrasive media disperses

Its minute, powder formula was listed in the table below 1.The composition of will filling a prescription carries out dispersion grinding with embodiment 3, but this routine rotating speed is 1900rpm, and blade diameter is 60mm, and grinding the cell body machine is 600ml, and milling time is 29 hours.

Comparative example 2 lmm zirconia material abrasive medias disperse

Its minute, powder formula was listed in the table below 1.The composition of will filling a prescription carries out dispersion grinding with embodiment 3, but this routine rotating speed is 1650rpm, and blade diameter is 50mm, and grinding the cell body machine is 600ml, and milling time is 55 hours.

Close the purity measurement that the slurry emission spectrometer carries out the branch lively stock with the induction lotus root, to detect the content that divides metal ingredient in the lively stock, know abrasive media after the collision of vigorous stirring, wearing and tearing of abrasive media trace or the pollution condition that grinding groove is worn and torn, following table 2 is its testing result.

Table 1

Illustration	Pigment content * (gram)	Dispersant	Disperse medium	Abrasive media
					Embodiment 3	42.16	Syn Fac 8216 (Milliken)25.3g	Deionized water 143.2g	Precision glass ball (Class V), particle size range 53-45 μ m (MO-SCISpecialty Products, L.L.C.) 570.7g
Comparative example 1	28.3	Joncryl 678 (Johnson)28.3g	Deionized water 132.3g	The polystyrene material, average grain diameter 250 μ m (Glen-Mill) 243.1g
					Comparative example 2	28.3	Joncryl J678 (Johnson)34.0g	Deionized water 126.6g	Zirconia particle diameter 1mm (prompt Nangong department) 817.4g

* adopt Sunfast Quinacridone Pigment (the pigment redness 122 that sun Chemical company makes)

Table 2

	Embodiment 3 (GIM002)	Comparative example 1 (HCT029)	Comparative example 2 (DFS061)
				Abrasive media (diameter)	Glass 50 μm	PS 250μm	Zircon 1mm
Pigment weight content %	12.0	10.8
				Average grain diameter (nm)	13.6	47.3	68.6
Milling time (hrs)	20	29	55
				Metallics total amount (ppm)	448.49	444.3	900.69

Disperse with the dispersal device with embodiment 3 in the comparative example 2, the result shows that its metallic pollution exceeds more than the twice.Observe by minute lively stock, tangible precipitation is arranged at the product of comparative example 2 bottom after leaving standstill a couple of days, and the color of this precipitation is for to be all white with abrasive media, and comparative example 2 test results should be underestimated the effect (other test specimen there is no this precipitation and takes place) of this abrasive media in hence one can see that the table 2.By test result as can be known, when using pretreated glass grinding media to disperse with the present invention, less because of its particle diameter, the energy that decentralized medium is single is lower, so it is more inviolent to wear and tear, so the combination of itself and stainless steel dispersion slot has the branch lively stock effect of low metallic pollution.

Embodiment 4 dispersion liquids of the present invention are prepared into the comparison of ink-jet ink and tradition time micron pigment dispersion

When if lively stock is as the application of color jet-ink ink with this minute, generally can require the total content of calcium, magnesium, chlorine three ions must be less than below the 100ppm, the concentration of this three ion that the product of embodiment 3 obtains after the ion chromatograph test is respectively [Mg ²⁺]=46.61ppm, [Ca ²⁺]=14.87ppm, [Cl ^-]=16.64ppm, its summation is 78.13ppm, and this test to divide pigment concentration of lively stock be 12%, with the pigment content of general ink four times of differences are arranged approximately, therefore again after recipe configuration, its total content is the scope for allowing still.Using this kind abrasive media to carry out high-quality ink-jet as known from the above prints and disperses also for feasible with the pigment of ink.

With magenta pigments dispersion liquid of the present invention (nano-scale) and tradition time micron magenta pigments dispersion liquid, with dispersible pigment dispersion (the about 10%wt of pigment content) 4.08%, NMF (Diethyleneglycol) 10.42%, antiseptic 0.1%, all the other are the composition composition of deionized water, are mixed into ink for inkjet.Both all can use hot bubble type ink jet ink cartridges ejection, its characteristic that the listed difference of following table 3 is arranged.

Table 3

Characteristic	Dispersible pigment dispersion preparation of the present invention	Tradition time micron dispersion liquid preparation
			Viscosity (cps)	1.64	2.08
Surface tension (dyne/cm)	48	42
			PH	7.15	8.2
Particle diameter	19.6	102.2
			Color Concentrated degree	0.91	0.85

Do not block according to the higher surface tension of the inkjet, ink glassware for drinking water of process for dispersing of the present invention preparation, bigger, the low easy filtration of particle diameter in prescription regulation and control space as can be known and the color degree of saturation than characteristics such as height.

What embodiment 5 used that traditional color mixing pigment of the present invention carries out the colorant coating tradition color (dispersible pigment dispersion) of the synthetic skin of PU and output dispersion liquid of the present invention relatively is listed in the table below 4:

Table 4

		Tradition color (dispersible pigment dispersion)	Dispersible pigment dispersion of the present invention
				Outward appearance	High concentration	Pigment essence color, color depth is but still slightly muddy white, and look more unsaturated	The nearly black of pigment essence color, color is extremely saturated
Low concentration	Pigment essence color, tool is not transparent, slightly muddy white	The pigment essence color tool transparency, approximate dyestuff state
			Viscosity (cps)		Hundreds of is to tens thousand of	＜20
Average grain diameter		＞100nm～several microns					＜30nm

Unsaturated compared to traditional color color and luster muddiness, viscosity is high, and shortcoming such as particle diameter is big, dispersible pigment dispersion of the present invention presents that color is extremely saturated, tool is transparent, low, the particle diameter of viscosity pole is lower than advantages such as 30 nanometers simultaneously.

Traditional color mixing pigment of the present invention is carried out the colorant coating of the synthetic skin of PU, mix water-based PU resin (70%) with dispersible pigment dispersion (8%wt), and add a small amount of wetting agent (～1%) and moisture content, after mixing, with spreading rod it is coated on the grey PU leather, with 70 ℃ of oven dry 5min,, obtain the listed result of following table 5 at last with perusal.

Table 5

Pigment mixed weight ratio		Coating characteristic
				IW6540	Nano dye of the present invention	Hiding rare	Color saturation
100	0	Difference	Difference
				99	1	Excellent	Excellent
97	3	Excellent	Excellent
				95	5	Can	Can
90	10	Can	Can

IW6540 is the water-based general-purpose color of producing available from Datong District company.Add 1 to 3% pigment of the present invention as shown in Table 5, can make the hiding rare height of colorant coating and color saturation better good.

The foregoing description only is to give an example for convenience of description, and the interest field that the present invention advocated should be as the criterion so that claim is described certainly, but not only limits to the foregoing description.

Claims (15)

1, a kind of ultramicron dispersing and milling method is characterized in that, mainly may further comprise the steps:

(a) matrix, dispersant are mixed with the dispersion medium a mixture;

(b) provide once pretreated abrasive media, and this abrasive media is added in this mixture; Wherein this abrasive media is the glass marble of average grain diameter less than 100 μ m;

(c) grind this mixture; And

(d) this abrasive media is separated in this dispersion liquid.

2, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein this matrix is embarrassed soluble dye, pigment, had crystalline organic matter, macromolecule or medicament powder.

3, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein this dispersant is to be selected from a group that is made up of anionic, cationic, nonionic and polymer electrolyte interfacial agent and composition thereof.

4, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein this dispersion medium is to be selected from a group that is made up of water, saline solution, methyl alcohol, ethanol, butanols, hexane, ethylene glycol and composition thereof.

5, ultramicron dispersing and milling method according to claim 1 is characterized in that, should be to screen in water overflow mode through pretreated abrasive media wherein.

6, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein the average grain diameter of this abrasive media is between 50 to 100 μ m.

7, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein the density of this abrasive media is to 3g/cm between 1 ³Between.

8, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein to grind this mixture be to be ground to the average grain diameter of this matrix less than 100nm to step (C).

9, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein this abrasive media is a spherical shape.

10, ultramicron dispersing and milling method according to claim 1 is characterized in that, wherein grinding is to finish with a grinder, and this grinder also comprises a stainless steel mixing channel and a stirring vane.

11, ultramicron dispersing and milling method according to claim 1, it is characterized in that wherein this grinder is a kind of in air type grinder, roller grinder, ball mill, mixer grinder, vibration-type grinder, planetary-type grinding machine, sand mill or the ball mill.

12, ultramicron dispersing and milling method according to claim 1 is characterized in that, its operation pattern is batch, continous way or half batch.

13, ultramicron dispersing and milling method according to claim 1 is characterized in that, its be used to make color with pigment, coating with pigment, polymer with pigment or pigment for printing ink.

14. a color is characterized in that, mainly comprises:

0.1 to the pigment of 70 weight portions, wherein the average grain diameter of this pigment is less than 100nm;

0.1 dispersant to 30 weight portions; And

The water of 40 to 90 weight portions;

Wherein this pigment is with dispersant and disperses medium to mix; Through average grain diameter be ground to less than the glass marble of 100 μ m average grain diameter less than 100nm after; In this dispersion liquid, separate and get.

15, color according to claim 14 is characterized in that, wherein this dispersant is to be selected from a group that is made up of anionic, cationic, nonionic and polymer electrolyte interfacial agent and composition thereof.