CN100406527C - Black pigment ink for ink-jet printer and method for preparing the same - Google Patents
Black pigment ink for ink-jet printer and method for preparing the same Download PDFInfo
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- CN100406527C CN100406527C CNB2005101378865A CN200510137886A CN100406527C CN 100406527 C CN100406527 C CN 100406527C CN B2005101378865 A CNB2005101378865 A CN B2005101378865A CN 200510137886 A CN200510137886 A CN 200510137886A CN 100406527 C CN100406527 C CN 100406527C
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Abstract
The present invention relates to black pigment ink for ink-jet printers. Carbon black dispersion liquid is firstly made of 10 % to 30 % of carbon black, 0.1 % to 1.25% of amphoteric polymers, 0.1 % to 1.5 % of flatting agents, 10% to 30% of humectant, 0.05 % to 0.5 % of defoaming agents and deionized water through humectation, sand grind and dispersion, and then 20% to 33 % of the carbon black dispersion liquid, 0.05 % to 2 % of surface active agents, 5 % to 50% of humectant, 0.1 % to 2 % of pH modifying agents, 0.5% to 2 % of driers, 0.1% to 0.5 % of preservative, 0.1 % to 0.5 % of mold preventing agents, 0.01 % to 0.5 % of chelating agents, 0.1% to 2 % of resin and the deionized water are added to prepare the black pigment ink. The ink can be used for continuously printing, and the writing is clear and has the advantages of no printing breakage, no woolly grain, wear resistance and color deterioration resistance; after stored in the ink-jet printers for a week, the ink still has the effect when used again.
Description
Technical field:
What the present invention relates to is that ink-jet printer is used Pigment black chromatic ink field.
Background technology:
Along with the continuous development of computer technology and numeral science and technology, ink-jet printer is more and more accepted by users as a kind of extremely useful output equipment, and popularity rate also day by day improves, and makes family and office work more be tending towards convenient, efficient, standard.At present the main flow on the ink-jet market remains type of dye ink, and it has characteristics such as beautiful in colour, reduction ratio height, but its relatively poor waterproof and fast light ability make its application be subjected to certain limitation; And pigment ink has excellent waterproof light fastness because the waterproof of pigment own, so print or product that air brushing is come out also with regard to waterproof.In this, black ink shows more outstandingly.In ink for ink-jet printer, the market share of black ink is maximum.Even the file that prints with paint ink is stained with water at its printing surface, ink also can be spread and sunk in hardly and be dyed paper; Its photostabilization is strong, and fugitive color can not be used for printing the files of permanent preservation; And ink dried is fast, does not infiltrate in the paper and can realize duplex printing, reduces and prints cost.
Carbon black is most important black pigment, the tinting material of ink-jet is gone up substantially and all is to use carbon black, with carbon black as tinting material, just there is such problem, because its surface is oil loving, the bad dispersibility in water, the thing of shower nozzle can take place to stop up, in preservation, can generate condensation product, heterogeneous, to such an extent as to phenomenon such as can not use, therefore must be by adding the carbon black solution that dispersion agent or additive method obtain stably dispersing.
Modal dispersing method is exactly by traditional tensio-active agent carbon black to be disperseed under the effect of dispersing apparatus, though this method is simple, but because the dispersant molecule structure exists following limitation: (1) hydrophilic radical at the lower or nonpolar particle surface of polarity in conjunction with not firm, easily desorb and cause disperseing the flocculation again of back particle; (2) lipophilic group does not possess enough carbon chain lengths (generally being no more than 18 carbon atoms), therefore can not produce abundant space steric effect in dispersion system plays stabilization, if resulting dispersion liquid is used for ink for ink-jet print, layering, coacervation will be occurred for a long time, shower nozzle will be stopped up behind the last machine.
Also have a kind of more common dispersing method to realize the carbon black stable dispersion relatively is typically described in the US 6232369 by coat a kind of resin at carbon blacksurface.This is a kind of a kind of ink for ink-jet printer that contains aqueous medium, water-insoluble tinting material, polymeric dispersant, water-sol polymkeric substance, the water-sol uses as polymeric additive, mainly be acrylic acid or the like, its content is 0.1 to 20%, and the sooty solid content is 2.75% in the ink.Have such shortcoming with resin dispersion: because pitch dispersant combines with carbon blacksurface with its effect of expectation performance, therefore the amount of the resin that adds just must surpass and carbon blacksurface bonded amount, otherwise the dispersion effect that just can not obtain.For this reason, just will inevitably residual unnecessary pitch dispersant in the dispersion liquid, and ink at the shower nozzle place because volatilization, thereby make these hardening of resins stop up shower nozzles.In addition, behind the interpolation pitch dispersant, the viscosity of ink increases, and can not obtain stable ink and spray.
In October, 1996, No. 5749952, US and US 5830265 have delivered a kind of brand-new ink for ink-jet print colorant respectively, are called the giant molecule chromophoric group.Present this colorant provides in companies such as Cabot and Orient.The special feature of this colorant utilizes chemically modified or exchange of particles mode exactly, and general pigment is made negatively charged ion chromophoric group and cationic chromophore, to promote the water-soluble of pigment.With the sooty chemically modified is example, and so-called negatively charged ion chromophoric group is exactly to import carboxylate radical or sulfonate radical at general carbon blacksurface, and reaction forms the carbon black that the surface has the anionic functional group.Cationic chromophore then is to import ammonium functional group or phosphine functional group reacts at carbon blacksurface, shows and has cationic carbon black and form.The dispersion liquid of being made by this technology is called as self-dispersing system, and the relevant patent of sooty has US5554739, US5571311, US5609671 etc.By the ink for ink-jet printer colour density height of making from disperse black carbon, the ink stably dispersing, the probability that stops up shower nozzle is low very little, but it also has unavoidable shortcoming, it is poorer than the ink of working it out with ordinary method that is exactly water resistance and crocking resistance, both had been to add resin also not have too big raising.
Day disclosure special permission communique discloses a kind of like this trial 96 years No. 3498: with chlorine bleach liquor and carbon black reaction, commercially available carbon black is further carried out oxide treatment, utilize the method for carbon black oxidation to improve the hydroxy radical content of carbon blacksurface and improve the sooty wetting ability with this.Yet, owing to containing sodium particle and the chlorion that much uses in the dispersion liquid, when this dispersion liquid is used as ink, need first elimination reactant in this method as oxygenant, carry out purifying by modes such as reverse osmosis membrane and ultrafiltration then.In addition, owing to reach the oxide treatment of 12h under 100 ℃ high temperature, generate so have water-soluble corrosive acid, this is very disadvantageous for shower nozzle.
Summary of the invention:
In order to overcome the defective in the above-mentioned technology, the invention provides a kind of preparation method who uses amphipathic nature polyalcohol carbon black to be carried out dispersive technology and black pigment ink for ink-jet printer.
Purpose of the present invention can be achieved through the following technical solutions: the one, adopt sand milling technology, use EFKA-3570, the EFKA-3580 flow agent of commercially available amphipathic nature polyalcohol Solsperse20000 and Dutch EFKA company that commercially available carbon black is disperseed, obtain the good carbon black dispersion liquid of dispersing property; The 2nd, prepared the printer ink of stable injection.
Described amphipathic nature polyalcohol is meant a class specific polymers type pigment dispersing agent that grows up the 1980s, and its molecular structure can carry out particular design according to the character of different surface of pigments and the polarity of dispersion medium.Its molecular structure is made up of two portions, and a part is an anchoring group, and it can be adsorbed in surface of pigments securely with the form of combination of single-point chemical bond or multiple spot hydrogen bonded, prevents to come off.Common group has-R2 ,-NR3+ ,-C00H ,-COO
-,-SO
3H ,-SO
3 2-,-PO
4 2-, polyamine, polyvalent alcohol and polyethers etc.; Another part is a solvent chain, and it is the polymkeric substance long-chain with certain molecular weight, with dispersion medium good consistency is arranged, and common group has polyester, polyethers, Polyolefin and polyacrylic ester etc.Amphipathic nature polyalcohol can form the protective layer of tens nanometers in surface of pigments, stops reunion between the particle effectively by sterically hindered effect, improves the dispersing of pigments performance.
At present, amphipathic nature polyalcohol has had sophisticated product-feed on market, as the Solsperse 20000 of Shanghai three positive CH series hyper-dispersants, Henkel 760, ICI company.The SOLSPERSE series product of ICI company have wide influence on market.The SOLSPERSE series polymer is the polymkeric substance of 12-oxystearic acid, and polymkeric substance degree＞4 are amphipathic nature polyalcohols of a kind of polyester type.SOLSPERSE-20000 used in the present invention be very typical application in the polymkeric substance of pure water system, add-on is 1.00%～7.00% (is carbon black dispersion liquid 0.10～2.10%) of amounts of carbon black, is preferably 2.00%～5.00% (be carbon black dispersion liquid 0.30～1.25%).It is optimum value that dispersant dosage forms fine and close monomolecular adsorption layer with it on the pigment particles surface usually, this will depend on the specific surface area (BET) of dispersed solid particulate, in fact this numerical value is to determine with the lower-most point of discharge curve with amphipathic nature polyalcohol with dispersion system viscosity by test, dispersion agent too much can raise the cost, and influences quality product; Cross the action effect of arriving at least.
Flow agent can be selected the modified organic silicon oxygen alkane flow agent EFKA-3570 or the EFKA-3580 of Dutch EFKA company, and the former is fluorine-carbon modified siloxanes, and the latter is organically-modified siloxanes, and the flow agent consumption is 0.10～1.50%, is preferably 0.40～1.00%.The main effect of wetting agent is that the quickening sooty is wetting, drives the bubble of carbon blacksurface away.Wetting agent can be in the kinds such as glycol ether, triglycol, N-Methyl pyrrolidone, 2-Pyrrolidone, N,N-DIMETHYLACETAMIDE, glycerine 1～2 kind, is preferably glycol ether or glycerine, and its consumption is 10.00%～30.00%, is preferably 15.00%～25.00%.Defoamer adopts the organic silicon modified by polyether compounds, mainly is can suppress and eliminate the bubble that produces in sand grinding process, can be for Henkel KGaA company
The BYK024 of SN3 13, NXZ, NDW and Bi Ke company etc. are preferably SN313 or BYK024, and consumption is 0.05%～0.50%, is preferably 0.10%～0.20%.What carbon black was selected for use is the commercially available special burnt high-carbon black pigment in Shanghai, and the sand milling addition is 10.00%～30.00%, is preferably 15.00%～25.00%.
In the sand milling stage, the present invention adopts following screening formulation (being the quality percentage composition):
Carbon black 15.00～25.00
Amphiphilic polymers sooty 2.00～5.00
Flow agent 0.40～1.00
Wetting agent 15.00～25.00
Defoamer 0.10～0.20
The deionized water surplus
Wherein, described carbon black is the special burnt high-carbon black pigment in Shanghai; Amphiphilic polymers is SOLSPERSE-20000; Flow agent is EFKA-3570 or EFKA-3580; Wetting agent is a glycol ether; Defoamer is the SN313 of Henkel KGaA company or the BYK024 of Bi Ke company;
The sand milling stage can be used conventional grinding plant, the hybrid grinding machine that comprises shearing grinding machine, crushing type grinding machine or impact mill or have shearing and shock action simultaneously.Concrete can comprise high-speed stirring mulser, three-roll mill, horizontal sand mill etc., wherein horizontal sand mill preferably.What the present invention used is the bipyramid horizontal sand mill.
The stable zirconia enamel pearl of yttrium of the import that the sand milling medium adopts, diameter is preferably 0.8～1.0mm at 0.4～1.2mm.
The sand milling stage that forms dispersion liquid can be divided into for three steps and carry out: wetting, grind and disperse.
Wetting step is normally got rid of gas or other dirt of carbon blacksurface under the effect of wetting agent, in order to improve wetting efficiency and wetting effect, preferably by mechanical means the carbon black agglomerate before grinding separately, will accelerate wet processes like this.The present invention is mixed to join amphipathic nature polyalcohol, wetting agent, flow agent and deionized water in the emulsor, stirs 5～10 minutes, adds carbon black and defoamer then under agitation condition, continues to stir 20～30 minutes.
Process of lapping can reduce the sooty size.Carbon black forms relative loose granule aggregate usually, process of lapping can reduce their size effectively, and agglomerate is separated into independently particle, and more expose its surface, make that under the effect of wetting dispersing agent carbon black particle can very fast being dispersed in the liquid.Process of lapping is performed until the carbon black pellet diameter and arrives needed particle size range, this size depends on multiple factor, for example the type of character, employed grinding plant and the medium of sooty type and character, the dispersion agent that adopted and dispersion liquid flux and the residence time etc. in grinding plant.In the present invention, wet mix squeezed into carry out sand milling in the sand mill and disperse, the mixed solution at the discharge port place sand milling that circulates, the detection of taking a sample every 30 minutes during this reaches standard up to the carbon black pellet of discharging.The standard that the present invention sets be the median size of particle less than 130nm, the volume content of the following particle of 300nm is not less than 95% simultaneously, particle detection apparatus is the laser particle analyzer HPPS5001 of Britain Ma Erwen company.This dispersion process is controlled between 10～40 ℃ the temperature of outlet feed liquid by the flow of regulating water coolant, and the time of sand milling, generally per kilogram feed liquid 5～10 minutes, rotating speed was 1500 commentaries on classics/min.
In dispersion process, wetting evengranular being dispersed in the liquid, each particle or granule are all surrounded by enough polymeric dispersants, form stable carbon black dispersion liquid.This needs a process, so the dispersion liquid of sand milling after qualified need be placed 12h and carry out filter operation later on again.The present invention adopts three-stage filtration, and one-level filter to adopt is 5.0 microns deep layer filter core, and cascade filtration adopts is 1.0 microns deep layer filter core, and three-stage filtration adopts is 0.5 micron deep layer filter core.After the filtration, the mean particle size of dispersion liquid is between 110～125nm, and the following volume content of 300nm is not less than 99%.
Ink for ink-jet printer is composed of the following components usually: carbon black dispersion liquid, tensio-active agent, wetting Agent for Printing Inks, PH conditioning agent, siccative, mould inhibitor, sterilant, sequestrant and deionized water etc.
For reconciliation statement surface tension, raising ink and the wetting property of substrate material and the discharge stability of ink, can add nonionic, negatively charged ion, positively charged ion and amphoterics in the water-based jet ink of the present invention.
As nonionogenic tenside, just like tweens such as polyethylene oxide alkyl ethers, polyoxyethylene allylic alkylation allyl ethers, polyoxyethylene oxypropylene block copolymer, fluorine system, silicon systems.
As anion surfactant, just like soap, alkyl sulfuric ester salt, alkylaryl sulphonate, sulfonated alkyl naphathalene, dialkyl group sulfonic acid succinate etc.
As cats product, for example alkylamine salt, quaternary amine, alkyl imidazole salt etc. are arranged.
As amphoterics, for example alkyl betaine, alkyl amine oxide etc. are arranged.
Preferred surfactants can be that the acetylenic diols compound of ethoxylation is (as Surfynol series, the Dynol of Air Prod ﹠ Chem
TMSeries), 1～2 kind in organosilicon and fluorocarbon surfactant (as the Nonyl@ series of the E.I.Du Pont Company) kind.Be more preferably Surfynol420, Surfynol 440, Surfynol465, Surfynol 485, Dynol
TM604, the Zonyl of Du Pont
Among the FSO 1～2 kind, they generally account for 0.05～2.00% of ink quality, are preferably 0.10%～1.00%
Wetting Agent for Printing Inks is the low volatilization of some a water miscible high boiling points organic solvent.Suitable wetting Agent for Printing Inks has: propylene glycol, 1, ammediol, 1, the 4-butyleneglycol, the lower alkyl ether of glycerine, glycol ether, dipropylene glycol, polyoxyethylene glycol, polypropylene glycol, polyvalent alcohol, as glycol monomethyl methyl ether, single ethyl ether or single-butyl ether, triglycol single-butyl ether, the mixture of acid amides such as dimethyl formamide, N,N-DIMETHYLACETAMIDE and alpha-pyrrolidone, N-Methyl pyrrolidone etc. and two or more component.Be preferably glycol ether, glycerine, glycol monomethyl methyl ether, single ethyl ether or single-butyl ether, triglycol single-butyl ether, alpha-pyrrolidone, the mixture of N-Methyl pyrrolidone and two or more component.These aqueous solvents mainly play moisture-keeping function, can prevent stopped nozzles, and they not only can use separately but also can mix use, and total amount accounts for 5.00～50.00% of ink quality, preferably accounts for 10.00～30.00% of ink.
The pH value of ink is too high or too low all to be deleterious to printer head, generally is advisable between 7～10.To add some pH regulator agent as one sees fit for this reason, suitable reagent has amine, as thanomin, diethanolamine, trolamine, N, N-dimethylethanolamine or Diisopropylamine, alkalimetal oxide, for example lithium hydroxide, sodium hydroxide, potassium hydroxide, and ammoniacal liquor, 2-amino-1-propyl alcohol, N-methylmorpholine, N-ethylmorpholine etc.Be preferably thanomin, diethanolamine, trolamine and ammoniacal liquor, in paint ink, they should be preferably 0.20～1.00% 0.10～2.00% by normal content.
For the time of drying after the suitable raising ink jet, can add siccative.Suitable siccative can be in the kinds such as methyl alcohol, ethanol, Virahol, acetone 1～2 kind, and its consumption is generally 0.50～2.00%.
Mould inhibitor, sterilant can prevent that ink is mouldy and corrupt, can use dehydrated sodium acetate, sodium benzoate, 1,2-benzisothiazole-3-ketone, zinc pyridine sulfo--1-oxide compound etc. can also be selected commercially available sterilant KATHON LXE (east-Rhom and Hass) and Mergal K7 (gram Lay benefactor department), mould inhibitor SKANEM-8 (east-Rhom and Hass) and BCM (Xuzhou insecticide factory) for use.Its consumption is the 0.10-0.50% of ink.
Sequestrant can seal the metal ion in the ink, prevent the nozzle place have metal separate out with ink in insolubles separate out etc., can use the tetramine salt of two amine salt, ethylenediamine tetraacetic ethanamide of sodium salt (EDTA), the ethylenediamine tetraacetic ethanamide of ethylenediamine tetraacetic ethanamide, ethylenediamine tetraacetic ethanamide or oxyacetic acid etc.These materials account for the 0.10～0.50% better of ink, are preferably 0.05～0.20%.
Generally all adding a part of resin in paint ink, mainly is to improve the fastness to rubbing of ink and the glossiness of printing.These resins can be Resins, epoxy, acrylic resin etc., acrylic resin preferably, particularly water miscible styrene acrylic resin class, the acrylic resin of use represent to be selected from following monomer: the ester of vinylformic acid, methacrylic acid, acrylic acid ester and methacrylic acid.Concrete example can comprise: in the kinds such as methyl methacrylate, Jia Jibingxisuanyizhi, n-BMA, methacrylic acid 2-hydroxy ester, methacrylic acid 2-chloroethene ester 1～2 kind.The molecular-weight average of used resin generally between 2000～20000, is preferably 4000～10000, and consumption is in 0.10%～1.00% (solid resin content).The present invention adopts the styrene acrylic resin JONCRYL of commercial available Johnson Polymer company
586, JONCRYL
680, JONCRYL
56 and JONCRYL
58.JONCRYL
56 is JONCRYL of 27% solid content
586 solution, molecular-weight average 4600, acid number 108; JONCRYL
58 is the JONCRYL of 52% solid resin content
680 solution, molecular-weight average 4900, acid number 215.This two resinoid all is low-molecular-weight water-soluble phenylethene acrylic resin, can significantly improve ink wet colour fastness and fastness to rubbing.
JONCRYL
56 preparation technology and method are as follows:
Mass content %
JONCRYL
586 chip solid 27.0
N-propyl alcohol 13.5
Ammoniacal liquor, 28% 4.0
Deionized water 55.5
The water, n-propyl alcohol and the ammoniacal liquor that add 70～90 ℃ in airtight agitator begin to stir, and slowly add JONCRYL in batches
586 solids add following batch after treating to dissolve fully again, and the pH value is surveyed in the cooling back, and it is adjusted into 8.9～9.2, and sealing is preserved stand-by.
In addition, in order to improve the anti-uv-ray of ink, can add anti-UV reagent; In order to prevent that ink from bubbling, and can also add defoamer when circulating, moving or making ink.
In the ink allotment stage, the present invention adopts following screening formulation (be the quality percentage composition, wherein the content of resin is the content of amounting to into solid resin):
Carbon black dispersion liquid 20.00～33.00
Tensio-active agent 0.10～1.00
Wetting Agent for Printing Inks 10.00～30.00
PH regulator agent 0.20～1.00
Siccative 0.50～2.00
Sanitas 0.10～0.50
Mould inhibitor 0.10～0.50
Sequestrant 0.05～0.20
Resin 0.20～1.50
The deionized water surplus
Ink allotment scheme is as follows: under the normal temperature, get carbon black dispersion liquid some (are 5.0% calculating according to carbon black in the ink) and add in the agitator, under agitation condition, add tensio-active agent, wetting Agent for Printing Inks, siccative, resin, pH regulator agent, sequestrant, Antisepticize and mildew preventive and deionized water.Under 80～120 rev/mins stirrer, stir 2h, leave standstill 24h, successively use the filter element filtering of 1 μ m and 0.45 μ m, can obtain the black pigment ink for ink-jet print.
The outstanding advantage of black pigment ink for ink-jet printer of the present invention is: can print continuously and do not break, clear, full, the no burr of writing had both made in printer placement for some time again with still having as above-mentioned effect; The literal of printing is wear-resisting not to fade, and has both made on glossiness photo papers and has printed, and touches wiping with hand after several minutes and does not fade; Print file are put into water, and font does not also have the burr appearance after 10 minutes.
Specific embodiments:
Embodiment 1
With 0.5 part of amphipathic nature polyalcohol Solsperse20000 (ICI company, down together), 0.6 part EFKA3580,5 portions of glycol ethers, 15 parts of glycerine and 60.8 parts of deionized waters join in the emulsor, under 80～120 rev/mins rotating speed, stirred 7 minutes, under agitation condition, add 18 parts of high-carbon black pigment (Shanghai coking then, together following) and 0.1 part of defoamer SN313 (Henkel KGaA product, down together), continue to stir 20 minutes, wet mix squeezed into carry out sand milling in the sand mill and disperse, the discharging sand milling that circulates, carried out sampling Detection every 30 minutes, reach standard up to the carbon black pellet of discharging.Dispersion process is controlled between 10～40 ℃ the temperature of outlet feed liquid by the flow of regulating water coolant, and the time of sand milling, generally per kilogram feed liquid 5～10 minutes, rotating speed was 1500 rev/mins.The three layer depth metafiltration cores that qualified dispersion liquid carries out 5.0 microns, 1.0 microns and 0.5 micron filter.The mean particle size of the dispersion liquid after the filter is 112nm, and the following volume content of 300nm is 100%.
Table 1: embodiment 2～6
Embodiment 7
The carbon black dispersion liquid that in being furnished with the jar of agitator, adds preparation among 27.8 parts of embodiment 1, under 80～120 rev/mins stirring with 0.6 part of Surfynol485 (Air Prod ﹠ Chem), 0.25 part of Dynol
TM604 (Air Prod ﹠ Chem), 4 parts of triglycol monobutyl ethers, 18 portions of glycol ethers, 0.3 part of thanomin, 1.5 parts of Virahols, 0.15 part of KATHON LXE (ROHM AND HAAS), 0.2 part of SKANEM-8 (ROHM AND HAAS), 0.1 part of oxyacetic acid and 1.5 parts of JONCRYL
56 (Johnson Polymer) add successively, add 45.6 parts of deionized waters at last, continue to stir 2h, leave standstill 24h, use the filter element filtering of 1 μ m and 0.45 μ m afterwards, can obtain the pigment inkjet ink.
Table 2: embodiment 8～15
Annotate: Surfynol 465, EP810 are U.S. air company product;
Zonyl.FSO is E.I.Du Pont Company's fluorocarbon surfactant product;
Table 3: the performance test of ink
Wherein:
1, the shower nozzle situation is meant the shower nozzle state ink is printed the A4 common paper of 100 page of 5% fraction of coverage continuously at machine on the epsonC65 printer after, ▲ ▲ ▲ the expression shower nozzle is intact; ▲ ▲ expression shower nozzle slightly stops up; ▲ expression shower nozzle seriously stops up;
2, the situation of preserving moisture is meant ink nozzle situation after placing a week on the machine under switch-on regime,
The expression nozzle is intact;
Expression has a small amount of shower nozzle short-term, but it is intact to clean once the back;
Expression has a small amount of shower nozzle short-term, but could be intact after must cleaning several times;
3, the writing situation is meant the state of ink printed on the A4 common paper, and ★ ★ ★ represents that writing is clear, full; ★ ★ represents that writing slightly blurs, has obvious burr phenomena; ★ represents the writing poor effect;
4, crocking resistance is meant and prints the black color lump on glossy photo paper, with the wiping of finger tripe, sees the degree that stains of finger after 10 minutes.◆ ◆ ◆ expression is faded hardly, ◆ ◆ expression has trace to fade, ◆ expression is faded serious;
5, water resistance is meant printing character on common A4 paper, after 5 minutes paper is placed in the clear water, places and takes out after 10 minutes, sees whether the literal edge burr or blooming occur.● ● ● expression literal clear-cut margin, no burr phenomena, with the same before the immersion, ● ● there is slight oozing out and burr phenomena at expression literal edge, ● the expression burr phenomena is serious, and writing fogs.
Claims (6)
1. an ink-jet printer Pigment black chromatic ink contains carbon black, aqueous medium and polymeric dispersant, it is characterized in that pH value 7～10, and weight percent consists of:
Carbon black dispersion liquid 20.00～33.00
Tensio-active agent 0.05～2.00
Wetting Agent for Printing Inks 5.00～50.00
PH regulator agent 0.10～2.00
Siccative 0.50～2.00
Sanitas 0.10～0.50
Mould inhibitor 0.10～0.50
Sequestrant 0.01～0.50
Resin 0.10～2.00
The deionized water surplus
Wherein said tensio-active agent can be acetylenic diols compound S urfynol series, the Dynol of ethoxylation
TMIn series and the fluorocarbon surfactant Nonyl@ series 1～2 kind;
Described wetting Agent for Printing Inks is a propylene glycol, 1, ammediol, 1, the mixture of 4-butyleneglycol, glycerine, glycol ether, dipropylene glycol, polyoxyethylene glycol, polypropylene glycol, glycol monomethyl methyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, triglycol single-butyl ether, dimethyl formamide, N,N-DIMETHYLACETAMIDE, alpha-pyrrolidone, N-Methyl pyrrolidone and two or more component;
Described pH regulator agent is thanomin, diethanolamine, trolamine, N, N-dimethylethanolamine, Diisopropylamine, lithium hydroxide, sodium hydroxide, potassium hydroxide, 2-amino-1-propyl alcohol, N-methylmorpholine, N-ethylmorpholine and ammoniacal liquor;
Described siccative is 1～2 kind in methyl alcohol, ethanol, Virahol, the acetone;
Described sequestrant is the sodium salt of ethylenediamine tetraacetic ethanamide, ethylenediamine tetraacetic ethanamide, two amine salt of ethylenediamine tetraacetic ethanamide, the tetramine salt or the oxyacetic acid of ethylenediamine tetraacetic ethanamide;
Described resin is the polymkeric substance and the styrene acrylic resin of methyl methacrylate, methylbenzene olefin(e) acid ethyl ester, n-BMA, methacrylic acid 2-hydroxy ester, methacrylic acid 2-chloroethene ester, and molecular-weight average is 2000～20000; Measure with solid resin;
Described carbon black dispersion liquid is for being disperseed to get through grinding by carbon black, amphiphilic polymers, flow agent, wetting agent and defoamer, and its weight percent consists of:
Carbon black 10.00～30.00
Amphiphilic polymers 0.10～2.10
Flow agent 0.10～1.50
Wetting agent 10.00～30.00
Defoamer 0.05～0.50
The deionized water surplus
Wherein said amphiphilic polymers is the polymkeric substance of 12-oxystearic acid, and polymkeric substance degree＞4 are amphipathic nature polyalcohols of a kind of polyester type;
Described flow agent is fluorine-carbon modified siloxanes EFKA-3570 or organically-modified siloxanes EFKA-3580;
Described wetting agent is 1～2 kind in glycol ether, N-Methyl pyrrolidone, 2-Pyrrolidone, N,N-DIMETHYLACETAMIDE, the glycerine;
Described defoamer is organic silicon modified by polyether compounds: SN313, NXZ, NDW or BYK024.
2. the described ink-jet printer of root a tree name claim 1 Pigment black chromatic ink is characterized in that weight percent consists of:
Carbon black dispersion liquid 20.00～33.00
Tensio-active agent 0.10～1.00
Wetting Agent for Printing Inks 10.00～30.00
PH regulator agent 0.20～1.00
Siccative 0.50～2.00
Sanitas 0.10～0.50
Mould inhibitor 0.10～0.50
Sequestrant 0.05～0.20
Resin 0.20～1.50
The deionized water surplus
Wherein said tensio-active agent is Surfynol420, Surfynol440, Surfynol465, Surfynol485, Dynol
TM604, Zonyl
Among the FSO 1～2 kind;
Described wetting Agent for Printing Inks is the mixture of glycol ether, glycerine, glycol monomethyl methyl ether, single ethyl ether or single-butyl ether, triglycol single-butyl ether, alpha-pyrrolidone, N-Methyl pyrrolidone and two or more component;
Described pH regulator agent is thanomin, diethanolamine, trolamine and ammoniacal liquor;
Described resin is the water-soluble phenylethene acrylic resin.
3. the described ink-jet printer of root a tree name claim 1 Pigment black chromatic ink is characterized in that described carbon black dispersion liquid weight percent consists of:
Carbon black 15.00～25.00
Amphiphilic polymers 0.30～1.25
Flow agent 0.40～1.10
Wetting agent 15.00～25.00
Defoamer 0.10～0.20
The deionized water surplus
Wherein said carbon black is the special burnt high-carbon black pigment in Shanghai;
Described wetting agent is 1～2 kind in glycol ether, the glycerine;
Described defoamer is SN313 or BYK024.
4. the described ink-jet printer of root a tree name claim 2 Pigment black chromatic ink is characterized in that described resin is water-soluble phenylethene acrylic resin: JONCRYL
56 or JONCRYL
58; JONCRYL
56 is JONCRYL of 27% solid content
586 solution, molecular-weight average 4600, acid number 108; JONCRYL
58 is the JONCRYL of 52% solid resin content
680 solution, molecular-weight average 4900, acid number 215.
5. ink-jet printer is characterized in that preparation technology carries out in two steps with the method for making of Pigment black chromatic ink:
(1) preparation of carbon black dispersion liquid: raw materials used kind and weight percent proportioning are:
Carbon black 10.00～30.00
Amphiphilic polymers 0.10～2.10
Flow agent 0.10～1.50
Wetting agent 10.00～30.00
Defoamer 0.05～0.50
The deionized water surplus
Preparation process is: 1. wetting: amphipathic nature polyalcohol, wetting agent and flow agent and deionized water are mixed to join in the emulsor, stirred 5～10 minutes, add carbon black and defoamer then under agitation condition, continue to stir 20～30 minutes; 2. sand milling: wet mix squeezed into carry out sand milling in the sand mill and disperse, the mixed solution that discharge port the comes out sand milling that circulates, detected every 30 minutes during this time, up to the carbon black pellet of discharging reach standard be the median size of particle less than 130nm, the volume content of the following particle of 300nm is not less than 95% simultaneously; Dispersion process is controlled between 10～40 ℃ the temperature of outlet feed liquid by the flow of regulating water coolant, and the time of sand milling is that rotating speed was 1500 commentaries on classics/min every kg feed liquid 5～10 minutes; 3. disperse: dispersion liquid need be placed 12h and carry out three-stage filtration later on again: it is 5.0 microns deep layer filter core that one-level is filtered what adopt, cascade filtration adopts is 1.0 microns deep layer filter core, three-stage filtration adopts is 0.5 micron deep layer filter core, after the filtration, the mean particle size of dispersion liquid is between 110～125nm, and the following volume content of 300nm is not less than 99%;
(2) ink formulation: raw materials used kind and weight percent proportioning are:
Carbon black dispersion liquid 20.00～33.00
Tensio-active agent 0.05～2.00
Wetting Agent for Printing Inks 5.00～50.00
PH regulator 0.10～2.00
Siccative 0.50～2.00
Sanitas 0.10～0.50
Mould inhibitor 0.10～0.50
Sequestrant 0.01～0.50
Resin 0.10～2.00
The deionized water surplus
Preparation process is: under the normal temperature, getting carbon black dispersion liquid adds in the agitator, under agitation condition, add tensio-active agent, wetting Agent for Printing Inks, siccative, resin, pH regulator agent, sequestrant, Antisepticize and mildew preventive and deionized water, under 80～120 rev/mins stirrer, stir 2h, leave standstill 24h, successively with the filter element filtering of 1 μ m and 0.45 μ m, can obtain the black pigment ink for ink-jet print afterwards;
A kind of as in high-speed stirring mulser, three-roll mill, the horizontal sand mill of the sand mill that uses in the sand milling step, the sand milling medium adopts the stable zirconia enamel pearl of yttrium, and diameter is at 0.4～1.2mm.
6. ink-jet printer according to claim 5 is characterized in that with the method for making of Pigment black chromatic ink the sand mill that uses in the sand milling step is horizontal sand mill, and the sand milling medium adopts the stable zirconia enamel pearl of yttrium, and diameter is at 0.8～1.0mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNB2005101378865A CN100406527C (en) | 2005-12-29 | 2005-12-29 | Black pigment ink for ink-jet printer and method for preparing the same |
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| CNB2005101378865A CN100406527C (en) | 2005-12-29 | 2005-12-29 | Black pigment ink for ink-jet printer and method for preparing the same |
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| CN100406527C true CN100406527C (en) | 2008-07-30 |
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