CN101486859B - Black nano water dispersible pigment fluid dispersion using polyurethane - Google Patents
Black nano water dispersible pigment fluid dispersion using polyurethane Download PDFInfo
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- CN101486859B CN101486859B CN200810187578.7A CN200810187578A CN101486859B CN 101486859 B CN101486859 B CN 101486859B CN 200810187578 A CN200810187578 A CN 200810187578A CN 101486859 B CN101486859 B CN 101486859B
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Abstract
一种使用聚氨酯的黑色纳米水性颜料分散液，其特征在于它由黑色颜料C.I.P.B.7、聚氨酯类分散剂、杀菌剂及去离子水组成；所说的黑色纳米水性颜料分散液的粒径D50控制在40.0～150.0nm之间。制备方法为：将分散剂和去离子水混合于容器并搅拌，加入黑色颜料，用高速剪切机剪切0.5~8小时，然后进行循环研磨分散，每隔15分钟进行粒度检测，直到分散液的粒径达到要求。本发明的优越性在于：本发明具有优良的分散性及保存稳定性，通过机械把黑色颜料团聚物打碎打小，让分散剂锚固在颜料颗粒的表面，防止颜料颗粒彼此之间团聚，所制得的颜料分散液稳定性增加。A black nano water-based pigment dispersion using polyurethane is characterized in that it is made up of black pigment CIPB7, polyurethane dispersant, bactericide and deionized water; the particle diameter D50 of said black nano water-based pigment dispersion is controlled at Between 40.0 and 150.0nm. The preparation method is: mix the dispersant and deionized water in a container and stir, add black pigment, cut with a high-speed shear for 0.5-8 hours, then carry out circular grinding and dispersion, and measure the particle size every 15 minutes until the dispersion is The particle size meets the requirements. The advantage of the present invention is that: the present invention has excellent dispersibility and storage stability, and the black pigment aggregates are mechanically broken into small pieces, so that the dispersant is anchored on the surface of the pigment particles and prevents the pigment particles from agglomerating with each other. The stability of the prepared pigment dispersion is increased.
Description
(1) technical field:
The present invention relates to a kind of dispersible pigment dispersion, particularly a kind of black nano-water dispersible pigment dispersion that uses urethane and preparation method thereof.
(2) background technology:
The market share that present black water paint ink with the black pigment preparation accounts for ink-jet printing ink is very big, the black water paint ink is used in general text printing more, even because its printing surface of black water paint ink print text file has water, ink also can be spread and sunk in hardly and be dyed paper; Simultaneously the text photostabilization printed of black pigment ink is strong, is difficult for fading, so can prolonged preservation; Again because the black pigment particle rests on paper surface in the ink, can the infiltrate paper, can realize duplex printing, save and print cost.And the black dyes ink was performed poor at this three face always in the past, so the black water paint ink is progressively substituting the black dye ink.
Black nano-water dispersible pigment dispersion is the key of preparation black water paint ink, but will expect that the good black nano-water dispersible pigment dispersion of dispersiveness, storage stability is by no means easy.Compare with general pigment dyestuff, the very tiny and surperficial oleophylic of the particle of black pigment, bad dispersibility in water obtains comparatively difficulty of good dispersion, so black nano-water dispersible pigment dispersion very easily goes wrong in preservation and use.In general, the mechanism of microcosmic particle stably dispersing can be divided into two kinds: the one, and electrocharge effect, electrocharge effect are the electric charges that utilizes the black pigment surface to exist, and make between the black pigment particle and produce electrical charge rejection, and the interparticle reunion of black pigment is alleviated; The 2nd, space steric effect.Space steric effect is to utilize the method for chemistry or physics to make the sterically hindered big segment of black pigment surface anchoring, utilizes the segmental space steric effect, and the interparticle reunion of black pigment is alleviated.If with enough mechanical energy the black pigment aggregate is smashed for a short time, allow dispersion agent be anchored at the surface of granules of pigments, prevent that granules of pigments from reuniting each other, so prepared dispersible pigment dispersion stability increases.
(3) summary of the invention:
The objective of the invention is to design a kind of black nano-water dispersible pigment dispersion that uses urethane and preparation method thereof, it is the good novel dispersion liquid preparation method of a kind of dispersiveness, storage stability.
Technical scheme of the present invention: a kind of black nano-water dispersible pigment dispersion that uses urethane is characterized in that it is made up of black pigment C.I.P.B.7, polyurethanes dispersion agent, sterilant and deionized water; Wherein the weight percent of black pigment C.I.P.B.7 is 3～30%, and the weight percent of polyurethanes dispersion agent is 5～50%, and the weight percent of sterilant is 0.2%, and surplus is a deionized water; The ratio of said black pigment and dispersion agent is between 0.5 ~ 3, and said polyurethanes dispersion agent is got the Solsperse 46000 of Lu Borun (Lubrizol) company; The particle diameter D of said black nano-water dispersible pigment dispersion
50Be controlled between 40.0～150.0nm.
The per-cent preferred 8 ~ 15% that above-mentioned said black pigment accounts for the dispersion liquid gross weight.
The per-cent preferred 9.2 ~ 17.3% that above-mentioned said polyurethanes dispersion agent accounts for the dispersion liquid gross weight.
Between the ratio preferred 1.1 ~ 1.8 of above-mentioned said black pigment and dispersion agent effective constituent.
Above-mentioned said black pigment is selected MA-7, MA100 or #40, the Special black 4 of Degussa (Degussa) company and the Raven 3500 of Colombia's chemistry (Columbian Chemical) company of Mongul-L, the R400R of Cabot (Cabot) company and R330R, Mitsubishi Chemical (Mitsubishi Chemical Corporation) company for use.
Above-mentioned said polyurethanes dispersion agent is through the neutralizing treatment of ammonium salt, molecular weight 2000 ~ 20000, preferred 4000 ~ 10000, wherein urethane contains polyethylene oxide, 2,2-dimethylol propionic acid and isophorone diisocyanate or 4,4-dicyclohexyl methane diisocyanate or 4,4-diphenylmethanediisocyanate.
Above-mentioned said sterilant is the benzisothiazole letones, selects the NipacideBIT-20 of Clariant (Clariant) company for use.
A kind of preparation method who uses the black nano-water dispersible pigment dispersion of urethane is characterized in that comprising the preparation of dispersion liquid and the preparation of ink, wherein:
(1) preparation of dispersion liquid may further comprise the steps:
1. dispersion agent and deionized water are mixed in the container according to aforementioned proportion, and stir;
2. add black pigment in proportion, fully wetting;
3. with high-speed shearing machine with the 2. dispersion liquid high speed shear 0.5～8.0 hour of gained of step, rotating speed is 1000～10000rpm, shears and finishes back placement 10.0～20.0 minutes;
4. with step 3. the shearing dispersion liquid of gained pump into and grind dispersion in the shredder;
5. with step 4. in the dispersion liquid of shredder discharge port gained enter the stock chest of shredder, pump into shredder once more and carried out circular grinding 0.5～24.0 hour;
6. in the process of lapping, adopted the LB-550 type dynamic laser look particle size analyzer that looses to carry out granularity Detection every 15 minutes, reach requirement up to the particle diameter of dispersion liquid.
The process of the dispersion liquid formulate ink that (two) makes is: get the 6. prepared dispersion liquid 10～50% of above-mentioned steps by weight percentage, wetting Agent for Printing Inks 5～30%, tensio-active agent 0.1～2% with the surplus deionized water, make ink for ink-jet print;
The said ink of making can be used in the Detection of Stability under the regular constant temperature of dispersion liquid.
Above-mentioned steps is 1.-3. for shearing dispersion steps: wherein mainly to act on be to make the dispersion agent dispersion and emulsion even to the high speed shear of step in 3., smash in the part black pigment than macroparticle, but its effect of overlong time is no longer remarkable, so preferred 1.0～2.0 hours of shear time.
Above-mentioned steps is 4.-6. for grinding dispersion steps: wherein the shredder of step in 4. be pin bar type shredder, ball mill and novel nano performance shredder-
A kind of among the-MILL NPM, grinding medium adopts a kind of in zirconium pearl, zirconium oxide bead and the high-performance silicic acid zirconium pearl, and mean diameter is between 0.05～1.00mm; Preferred rotating speed is pin bar type shredder and the zirconium oxide bead of diameter between 0.05～0.20mm of 600～4000rpm; The grinding purposes of said step in 4. is to make the particle diameter of black nano-water dispersible pigment dispersion continue to reduce, but prolongation along with milling time, its particle diameter lowering speed will be far smaller than initial 1.0～3.0 hours, and grinding effect is no longer remarkable, so preferred 1.0～3.0 hours of milling time; The discharge port temperature of said step in 5. is controlled between 20～40 ℃; 6. said step is the pigment granularity Detection.
The step of the pigment granularity Detection of above-mentioned said step in 6. is:
A, take out a testing sample with dropper, put into the test tube that specification is 18mm * 180mm, add deionized water height to 1/2 test tube height, vibration shakes up;
B, the sample that will dilute are put into the ultrasonic 2mins of ultrasonic instrument, and frequency setting is 40kHz * 80%, and temperature is 25 ℃;
C, put into the sample of ultrasonic mistake respectively in 3 cuvettes, liquid level is lower than cuvette outer 0.5cm;
LB-550 application program on d, the double-click computer desktop;
E, open the lid of LB-550 type dynamic light scattering nano particle size analyser gently, in sample pool, put into the cuvette that fills sample;
F, click Temp Panel, treat that temperature controls to 25 ℃ after, click Meas.Panel, Measurement Panel appears on the screen and after, click Measure, begin test;
G, the test of wait machine finish record data.The particle diameter of each sample is the weighted mean of three observed values.
Superiority of the present invention is: the present invention has good dispersiveness and storage stability, smash the black pigment aggregate little by machinery, allow dispersion agent be anchored at the surface of granules of pigments, prevent that granules of pigments from reuniting each other, prepared dispersible pigment dispersion stability increases.
Annotate: D
50: the cumulative particle sizes volume of distribution percentage ratio of a sample reaches 50% o'clock pairing particle diameter.
(4) embodiment:
In this case about the explanation of the effective content of dispersion agent: the effective content of dispersion agent is got the reference numerals on this commercial dispersants product description, dispersion agent Solsperse 46000 with Lu Borun (Lubrizol) company is an example, Solsperse46000 is the aqueous high molecular dispersion agent, and effective content is 50%.It is fixed that the consumption of this dispersion agent comes according to the specific surface area of black pigment, the black pigment of the general every 1m2/g of specific surface area need add the Solsperse44000 that contains the 2.5mg effective content, along with the minimizing of nano particle diameter, also can take the circumstances into consideration to add dispersion agent according to circumstances to improve dispersion effect.Black pigment adopts the MA-7 of Mitsubishi Chemical (Mitsubishi Chemical Corporation), and its initial particle is 24nm, specific surface area 115m2/g.
For the testing product quality, following experiment testing process to product property is arranged:
Month stability experiment of normal temperature:
Testing sample is put into Glass Containers, in the environment of constant temperature (25 ℃) constant humidity (35%RH), placed one month, measure the change of granularity situation of a month front and back sample.
Accelerated tests:
Testing sample is put into Glass Containers, after in 60 ℃ constant temperature oven, preserving for two weeks, making it timeliness and promote, measure the change of size of sample before and after the timeliness.
Frozen process experiment:
Testing sample is put into-20 ℃ refrigerator and taken out the baking oven one day of putting into 50 ℃ after one day.3 times so repeatedly.The change of size of sample before and after measuring.
" part " among the embodiment by weight.
Embodiment 1
Black pigment MA-7 with 8 parts of Mitsubishi Chemicals (Mitsubishi Chemical Corporation), 9.2 the dispersion agent Solsperse 46000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.2 mixing with the high speed shear agitator, the sterilant Nipacide BIT-20 of part Clariant (Clariant) company and 82.6 parts of deionized waters after evenly, must shear dispersion liquid in 1 hour, shearing dispersion liquid to 300g ground 1 hour in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The ratio of pigment and dispersion agent is 1.74: 1.With the preparation water dispersible pigment dispersion at room temperature, under 60 ℃, carry out STABILITY MONITORING; The water dispersible pigment dispersion of preparation is carried out freeze-thaw cycle experiment.
Comparative example 1
Black pigment MA-7 with 8 parts of Mitsubishi Chemicals (Mitsubishi Chemical Corporation), 0.2 mixing with the high speed shear agitator, the sterilant Nipacide BIT-20 of part Clariant (Clariant) company and 91.8 parts of deionized waters after evenly, must shear dispersion liquid in 1 hour, shearing dispersion liquid to 300g ground 1 hour in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.With the preparation water dispersible pigment dispersion at room temperature, under 60 ℃, carry out STABILITY MONITORING; The water dispersible pigment dispersion of preparation is carried out freeze-thaw cycle experiment.
Comparative example 2
Black pigment MA-7 with 8 parts of Mitsubishi Chemicals (Mitsubishi Chemical Corporation), 9.2 the dispersion agent Solsperse 44000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.2 mixing with the high speed shear agitator, the sterilant Nipacide BIT-20 of part Clariant (Clariant) company and 82.6 parts of deionized waters after evenly, must shear dispersion liquid in 1 hour, shearing dispersion liquid to 300g ground 1 hour in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The ratio of pigment and dispersion agent is 1.74: 1.With the preparation water dispersible pigment dispersion at room temperature, under 60 ℃, carry out STABILITY MONITORING; The water dispersible pigment dispersion of preparation is carried out freeze-thaw cycle experiment.
Comparative example 3
Carbon black MA-7 with 8 parts of Mitsubishi Chemicals (Mitsubishi Chemical Corporation), 19.2 the dispersant B orchi Gen SN 95 of part bright Sheng (LANXESS Corporation) company, 0.2 mixing with the high speed shear agitator, the sterilant Nipacide BIT-20 of part Clariant (Clariant) company and 72.6 parts of deionized waters after evenly, must shear dispersion liquid in 1 hour, shearing dispersion liquid to 300g ground 1 hour in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The ratio of pigment and dispersion agent is 1.67: 1.With the preparation water dispersible pigment dispersion at room temperature, under 60 ℃, carry out STABILITY MONITORING; The water dispersible pigment dispersion of preparation is carried out freeze-thaw cycle experiment.
The black nano-water dispersible pigment dispersion prescription of table 1 embodiment 1 and comparative example 1 ~ 3 and the ratio of pigment and dispersion agent
| Dispersion agent | Black pigment amount/w% | Disperse dosage/w% | Pigment: dispersion agent | |
| Comparative example 1 | Do not have | 8 | 0 | NA |
| Comparative example 2 | Solsperse?44000 | 8 | 9.2 | 1.74∶1 |
| Comparative example 3 | Borchi?Gen SN-95 | 8 | 19.2 | 1.67∶1 |
| Embodiment 1 | Solsperse?46000 | 8 | 9.2 | 1.74∶1 |
The changing conditions of particle diameter D50 (nm) after January of black nano-water dispersible pigment dispersion under table 2 normal temperature
| Dispersion agent | Grind the back particle diameter | Normal temperature particle diameter after following January | Particle diameter after the accelerated tests | Particle diameter behind the frozen process experiment | |
| Comparative example 1 | Do not have | NA | ?NA | NA | NA |
| Comparative example 2 | Solsperse 44000 | 91.2 | ?89.3 | 110.5 | 106.1 |
| Comparative example 3 | Borchi?Gen SN-95 | 93.8 | ?90.8 | Layering | 107.6 |
| Embodiment 1 | Solsperse 46000 | 97.8 | ?95.5 | 89.4 | 96.7 |
Change of size after table 3 embodiment and comparative example stability experiment, frozen process experiment and the accelerated tests
| Dispersion agent | Room temperature is the change of size rate after following January | Change of size rate behind the frozen process experiment | Change of size rate after the accelerated tests | |
| Comparative example 1 | Do not have | NA | NA | NA |
| Comparative example 2 | Solsperse 44000 | -2.1％ | 0.3％ | 21.1％ |
| Comparative example 3 | Borchi?Gen SN-95 | -3.2％ | 14.7％ | Layering |
| Embodiment 1 | Solsperse 46000 | -2.4％ | -1.9％ | -8.5％ |
Comparative example 1 is sheared the back gained and is sheared dispersion liquid and can not circulate and enter shredder and grind, comparative example 2 and comparative example 3 gained dispersion liquid normal temperature are stable in next month, but behind process accelerated tests and the frozen process experiment but is not very stable, after the comparative example 2 gained dispersion liquid accelerated tests particle size growth 21.1%, layering after the comparative example 3 gained dispersion liquid accelerated tests.In the embodiment 1 gained dispersion liquid one month at normal temperatures, after the accelerated tests and frozen process experiment after storage stability good.
Claims (10)
1. black nano-water dispersible pigment dispersion that uses urethane is characterized in that it is made up of black pigment C.I.P.B.7, polyurethanes dispersion agent, sterilant and deionized water; Wherein the weight percent of black pigment C.I.P.B.7 is 8～15%, and the weight percent of polyurethanes dispersion agent is 9.2～17.3%, and the weight percent of sterilant is 0.2%, and surplus is a deionized water; The ratio control of said black pigment and dispersion agent effective constituent is between 1.1～1.8, and said polyurethanes dispersion agent is got the Solsperse46000 of Lu Borun (Lubrizol) company; The particle diameter D of said black nano-water dispersible pigment dispersion
50Be controlled between 40.0～150.0nm.
2. according to the said a kind of black nano-water dispersible pigment dispersion that uses urethane of claim 1, it is characterized in that said black pigment is the MA-7 of Mitsubishi Chemical (MitsubishiChemical Corporation) company.
3. according to the said a kind of black nano-water dispersible pigment dispersion that uses urethane of claim 1, it is characterized in that the neutralizing treatment of said polyurethanes dispersion agent through ammonium salt, molecular weight 2000～20000, wherein urethane contains polyethylene oxide, 2,2-dimethylol propionic acid, isophorone diisocyanate or polyethylene oxide, 2,2-dimethylol propionic acid, 4,4-dicyclohexyl methane diisocyanate or polyethylene oxide, 2,2-dimethylol propionic acid, 4, the 4-diphenylmethanediisocyanate.
4. according to the said a kind of black nano-water dispersible pigment dispersion that uses urethane of claim 1, the molecular weight that it is characterized in that said polyurethanes dispersion agent is 4000～10000.
5. according to the said a kind of black nano-water dispersible pigment dispersion that uses urethane of claim 1, it is characterized in that said sterilant is the benzisothiazole letones, select the Nipacide BIT-20 of Clariant (Clariant) company for use.
6. preparation method according to the black nano-water dispersible pigment dispersion of the said use urethane of claim 1, its preparation process feature is as follows:
1. with dispersion agent and deionized water according to the described mixed of claim 1 in container, and stir;
2. add black pigment and sterilant according to the described ratio of claim 1, fully wetting;
3. with high-speed shearing machine with the 2. dispersion liquid high speed shear 0.5～8.0 hour of gained of step, rotating speed is 1000～10000rpm, shears and finishes back placement 10～20 minutes;
4. with step 3. the shearing dispersion liquid of gained pump into and grind dispersion in the shredder;
5. with step 4. in the dispersion liquid of shredder discharge port gained enter the stock chest of shredder, pump into shredder once more and carried out circular grinding 0.5～24.0 hour.
7. according to the preparation method of the said a kind of black nano-water dispersible pigment dispersion of claim 6, it is characterized in that during said step 3. with high-speed shearing machine the 2. dispersion liquid high speed shear 1～2 hour of gained of step.
8. according to the preparation method of the said a kind of black nano-water dispersible pigment dispersion of claim 7, it is characterized in that shredder during said step 4. be pin bar type shredder, ball mill and nanometer performance shredder-
Among-MILL the NPM any, grinding medium adopts the zirconium pearl, and mean diameter is between 0.05～1.00mm.
9. the preparation method of said a kind of black nano-water dispersible pigment dispersion according to Claim 8 is characterized in that zirconium pearl that grinding medium adopts is any in zirconium oxide bead and the zirconium silicate pearl.
10. the preparation method of said a kind of black nano-water dispersible pigment dispersion according to Claim 8, it is characterized in that said shredder is a pin bar type shredder, its rotating speed is 600～4000rpm, and grinding medium adopts the zirconium oxide bead of diameter between 0.05～0.20mm.
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|---|---|---|---|
| CN200810187578.7A CN101486859B (en) | 2007-12-28 | 2008-12-26 | Black nano water dispersible pigment fluid dispersion using polyurethane |
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|---|---|---|---|
| CN200710060600 | 2007-12-28 | ||
| CN200710060600.7 | 2007-12-28 | ||
| CN200810187578.7A CN101486859B (en) | 2007-12-28 | 2008-12-26 | Black nano water dispersible pigment fluid dispersion using polyurethane |
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| CN101486859B true CN101486859B (en) | 2011-08-31 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2012039716A1 (en) | 2010-09-23 | 2012-03-29 | Hewlett-Packard Development Company, L.P. | Ink jet ink with high structure pigment particles |
| CN104262570B (en) * | 2014-09-16 | 2016-08-17 | 中国科学技术大学 | A kind of preparation method of black water polyurethane dyestuff |
| CN104878463B (en) * | 2015-06-08 | 2016-09-07 | 连云港杜钟新奥神氨纶有限公司 | A kind of hyper-dispersant and the preparation method without dye polyurethane elastomeric fiber |
| CN111718619A (en) * | 2020-05-25 | 2020-09-29 | 浙江大利实业有限公司 | Production process of water-based environment-friendly nubuck black paste |
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