CN101597443A - A kind of Yellow nanometer water-type pigment dispersion - Google Patents
A kind of Yellow nanometer water-type pigment dispersion Download PDFInfo
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- CN101597443A CN101597443A CN 200810154435 CN200810154435A CN101597443A CN 101597443 A CN101597443 A CN 101597443A CN 200810154435 CN200810154435 CN 200810154435 CN 200810154435 A CN200810154435 A CN 200810154435A CN 101597443 A CN101597443 A CN 101597443A
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Abstract
A kind of Yellow nanometer water-type pigment dispersion, it is characterized in that it is made up of yellow ultramarine, polymer block polymer type dispersion agent, wetting Agent for Printing Inks and deionized water, it accounts for total weight percent and is respectively 3～30%, 5～50% and 3～30%, and surplus is a deionized water; The particle diameter D of said magenta nanometer water-type pigment dispersion
50Be controlled between 40.0～150.0nm.Preparation method: dispersion agent and deionized water are mixed in container and stir, add yellow ultramarine, sheared 0.5～8 hour, carry out circular grinding then and disperse, carried out granularity Detection every 15 minutes, reach requirement up to the particle diameter of dispersion liquid with high-speed shearing machine.The Yellow nanometer water-type pigment dispersion that has added wetting Agent for Printing Inks after high cold cycle and high temperature quicken, its particle diameter D
50Variation per-cent less than 50%, improved its stability under high cold cycle and high temperature acceleration environment, and it had no adverse effects in the stability under the normal temperature condition.
Description
(1) technical field:
The present invention relates to a kind of dispersible pigment dispersion, particularly a kind of Yellow nanometer water-type pigment dispersion that is used as the ink-jet field and preparation method thereof.
(2) background technology:
The yellow ink that spray ink Printing is in the market used can be divided into yellow dyes type ink and yellow ultramarine type ink, and the dyestuff in the yellow dyes type ink is to exist with molecularity, thus obtained printed matter clear picture, but fade easily and poor water resistance.Pigment in the yellow ultramarine type ink is to exist with graininess, and thus obtained printed matter has advantages such as fast light, water-fast, so the yellow ultramarine ink is progressively substituting the yellow dyes ink.Because the stability of Yellow nanometer water-type pigment dispersion is significant to its application, so in the preparation of yellow ultramarine ink, the most key to prepare stable Yellow nanometer water-type pigment dispersion, its difficult point is the super-refinement of yellow ultramarine particle, the homogenizing of size distribution and the stability of Yellow nanometer water-type pigment dispersion.Because yellow ultramarine particle particularly nano level yellow ultramarine particle has bigger specific surface area and higher surface energy, very easily produce spontaneous cohesion and agglomeration each other, form the bigger primary particle of particle diameter, thereby make the stability decreases of Yellow nanometer water-type pigment dispersion, in general obtain disperseing under the normal temperature more stable Yellow nanometer water-type pigment dispersion by the method for adding dispersion agent, but Yellow nanometer water-type pigment dispersion is unstable under the big condition of high temperature and the temperature difference, easily layering makes troubles for the transportation of Yellow nanometer water-type pigment dispersion.Therefore develop high temperature resistant and high-low temperature resistant round-robin Yellow nanometer water-type pigment dispersion is very necessary to solve a transportation difficult problem.
(3) summary of the invention:
The objective of the invention is to design a kind of Yellow nanometer water-type pigment dispersion, it by add wetting Agent for Printing Inks make Yellow nanometer water-type pigment dispersion under the high low temperature cycling condition and the stability under the high temperature acceleration environment improve, and can not influence pigment dispersion system stability at normal temperatures, solve the difficult problem of Yellow nanometer water-type pigment dispersion transportation.
Technical scheme of the present invention: a kind of Yellow nanometer water-type pigment dispersion, it is characterized in that it is made up of yellow ultramarine, polymer block polymer type dispersion agent, wetting Agent for Printing Inks and deionized water, wherein yellow ultramarine accounts for 3～30% of total weight percent, polymer block polymer type dispersion agent accounts for 5～50% of total weight percent, wetting Agent for Printing Inks accounts for 3～30% of total weight percent, and surplus is a deionized water; Said wetting Agent for Printing Inks is n-propyl alcohol, ethylene glycol, 1,2-propylene glycol, 1, ammediol, 1,4-butyleneglycol, 1,2-pentanediol, 1,5-pentanediol, glycerol, 1,2, at least a in the above high boiling point of 6-hexanetriol, Diethylene Glycol, Triethylene glycol, poly(oxyethylene glycol) 400 and Polyethylene Glycol-600, the difficult volatilization alcohols; The particle diameter D of said Yellow nanometer water-type pigment dispersion
50Be controlled between 40.0～150.0nm.
Above-mentioned said compositing formula can also comprise sterilant, and its weight percent that accounts for the dispersion liquid gross weight is 0.0～0.2%.
Above-mentioned said yellow ultramarine is selected the C.I. Pigment Yellow 73 74 of Switzerland vapour Bagong department (Ciba) for use.
Above-mentioned said polymer block polymer type dispersion agent is selected the SOLsperse 43000 of U.S. Lubrizol Corp. (Lubrizol) for use.
Above-mentioned said wetting Agent for Printing Inks is preferred 1,2-propylene glycol, 1, ammediol, 1,4-butyleneglycol, 1,2-pentanediol, 1, the combination of one or more in the 5-pentanediol.
Above-mentioned said sterilant is 1, and the 2-benzisothiazole-3-ketone is got the Nipacide BIT-20 of Clariant company (Clariant).
A kind of preparation method of Yellow nanometer water-type pigment dispersion 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 liquid, wetting Agent for Printing Inks and deionized water are mixed in the container according to aforementioned proportion, and stir;
2. add yellow ultramarine 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,
After finishing, shearing placed 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, preferred 1.0～3.0 hours;
6. in the process of lapping, adopted the 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% and surplus deionized water are made 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 yellow ultramarine than macroparticle, but its effect of overlong time is no longer remarkable, so preferred 1.0～2.0 hours of shear time.
Step 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, mean diameter is between 0.05～1.00mm, and preferred rotating speed is pin bar type shredder and the zirconium oxide bead of diameter between 0.05～0.20mm of 600～4000rpm; 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:
Compare dispersible pigment dispersion layering and the big situation of change of size per-cent after high cold cycle and high temperature quicken of no wetting Agent for Printing Inks, the Yellow nanometer water-type pigment dispersion that has added wetting Agent for Printing Inks is after high cold cycle and high temperature acceleration, the variation per-cent of its particle diameter D50 is less than 50%, improved its stability under high cold cycle and high temperature acceleration environment, and it has been had no adverse effects in the stability under the normal temperature condition.
Annotate: D50: the cumulative particle sizes volume of distribution percentage ratio of a sample reaches 50% o'clock pairing particle diameter.
(4) embodiment:
For the testing product quality, following experiment testing process to product property is arranged:
Test month stability experiment of 1. normal temperature:
Testing sample (the related Yellow nanometer water-type pigment dispersion of the present invention) is put into Glass Containers, in the environment of constant temperature (25 ℃) constant humidity (35%RH), placed one month, measure the particle diameter D of a month front and back sample
50Changing conditions.
Test 2. high low temperature circulation experiments:
Testing sample is put into Glass Containers, placed in the environment of 60 ℃ of high temperature 24 hours, take out then in the environment of low temperature-20 ℃ and placed 24 hours, this be an one-period, circulates altogether three cycles, and amounting to the time spent is 6 days, measures the particle diameter D of circulation front and back sample
50Changing conditions.
Test 3. high temperature accelerated tests:
Testing sample is put into Glass Containers, in the environment of 60 ℃ of high temperature, placed for 2 weeks, measure the particle diameter D50 changing conditions of 2 all front and back samples.
Embodiment 1:
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 the dispersion agent SOLsperse 43000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.20 the sterilant Nipacide BIT-20 of part Clariant (Clariant) company, 10.0 part wetting Agent for Printing Inks 1,2-propylene glycol and 69.8 parts of deionized waters mix with the high speed shear agitator must shear dispersion liquid in 1 hour after evenly, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Embodiment 2
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 the dispersion agent SOLsperse 43000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.20 the sterilant Nipacide BIT-20 of part Clariant (Clariant) company, 10.0 part wetting Agent for Printing Inks 1, ammediol and 69.8 parts of deionized waters mix with the high speed shear agitator must shear dispersion liquid in 1 hour after evenly, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Embodiment 3
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 the dispersion agent SOLsperse 43000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.20 the sterilant Nipacide BIT-20 of part Clariant (Clariant) company, 5.0 part wetting Agent for Printing Inks 1, ammediol, 5.0 parts of wetting Agent for Printing Inkss 1,4-butyleneglycol and 69.8 parts of deionized waters mix with the high speed shear agitator must shear dispersion liquid in 1 hour after evenly, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Embodiment 4
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 part road Bo Run (Lubrizol), the dispersion agent S0Lsperse 43000 of company, its active constituent content 50%, 0.20 the sterilant Nipacide BIT-20 of part Clariant (Clariant) company, 1.0 part wetting Agent for Printing Inks 1, ammediol, 1.0 part wetting Agent for Printing Inks 1, the 4-butyleneglycol, 8.0 part wetting Agent for Printing Inks 1,2 pentanediols and 69.8 parts of deionized waters mix with the high speed shear agitator must shear dispersion liquid in 1 hour after evenly, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Embodiment 5
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 the dispersion agent S0Lsperse 43000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.20 the sterilant NipacideBIT-20 of part Clariant (Clariant) company, 10.0 part wetting Agent for Printing Inks 1,5-pentanediol and 69.8 parts of deionized waters mix with the high speed shear agitator must shear dispersion liquid in 1 hour after evenly, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Comparative example 1
Yellow ultramarine C.I. Pigment Yellow 73 74 with 10.0 parts of Ciba companies, 10.0 the dispersion agent SOLsperse 43000 of part road Bo Run (Lubrizol) company, its active constituent content 50%, 0.20 mixing with the high speed shear agitator, the sterilant Nipacide BIT-20 of part Clariant (Clariant) company and 79.8 parts of deionized waters after evenly, must shear dispersion liquid in 1 hour, shearing dispersion liquid to 300.00g ground 2 hours in 0.14L volumetrical shredder again, obtained water dispersible pigment dispersion.The water dispersible pigment dispersion of preparation is carried out a month stability experiment, high low temperature circulation experiment and high temperature accelerated tests at normal temperatures.
Comparative example 2-6 is all according to the step and the following formulation ratio pigment preparation dispersion liquid of above-mentioned comparative example 1, and and embodiment carry out month stability experiment, high low temperature circulation experiment and a high temperature accelerated tests simultaneously.
The Yellow nanometer water-type pigment dispersion prescription of table 1 comparative example 2～4
The particle diameter D of table 2 Yellow nanometer water-type pigment dispersion
50Changing conditions
Dispersion agent is in the said comparative example:
Comparative example 1,2: dispersion agent Solsperse 43000 is U.S. Lubrizol Corp. (Lubrizol) product.
Comparative example 3,4: dispersion agent Solsperse 47000 is U.S. Lubrizol Corp. (Lubrizol) product.
As can be seen from the above table, embodiment 1-5 gained dispersion liquid, be to use dispersion agent SOLsperse 43000 and added the Yellow nanometer water-type pigment dispersion of wetting Agent for Printing Inks, pigment dispersion ties up to change of size per-cent under height temperature circulation and the high temperature acceleration environment less than 50.0%, and do not have demixing phenomenon, stability obviously improves, under normal temperature condition, change of size per-cent is little, illustrates that adding wetting Agent for Printing Inks does not have influence to the stability of with this understanding dispersion liquid; Comparative example 1,3 gained dispersion liquids have used the dispersion agent identical and different with embodiment respectively, are not all adding under the situation of wetting Agent for Printing Inks, and high cold cycle and high temperature layering and the big phenomenon of change of size per-cent occur after quickening; Comparative example 2 gained dispersion liquids have used dispersion agent identical with embodiment and different wetting Agent for Printing Inkss, and high temperature demixing phenomenon also occurs after quickening; The dispersion liquid of comparative example 4 gained has used dispersion agent different with embodiment 1 and identical wetting Agent for Printing Inks, and high temperature quickens back change of size per-cent greater than 50.0%, and experimental result is undesirable.Reach a conclusion thus, under the situation of using specific dispersant, in the yellow ultramarine dispersion liquid, add specific wetting Agent for Printing Inks and help obtaining high-low temperature resistant circulation and the resistant to elevated temperatures stable dispersions that is easy to transport.
Claims (9)
1. Yellow nanometer water-type pigment dispersion, it is characterized in that it is made up of yellow ultramarine, polymer block polymer type dispersion agent, wetting Agent for Printing Inks and deionized water, wherein yellow ultramarine accounts for 3～30% of total weight percent, polymer block polymer type dispersion agent accounts for 5～50% of total weight percent, wetting Agent for Printing Inks accounts for 3～30% of total weight percent, and surplus is a deionized water; Said wetting Agent for Printing Inks is n-propyl alcohol, ethylene glycol, 1,2-propylene glycol, 1, ammediol, 1,4-butyleneglycol, 1,2-pentanediol, 1,5-pentanediol, glycerol, 1,2, at least a in the above high boiling point of 6-hexanetriol, Diethylene Glycol, Triethylene glycol, poly(oxyethylene glycol) 400 and Polyethylene Glycol-600, the difficult volatilization alcohols; The particle diameter D50 of said Yellow nanometer water-type pigment dispersion is controlled between 40.0～150.0nm.
2. according to the said a kind of Yellow nanometer water-type pigment dispersion of claim 1, it is characterized in that the compositing formula of dispersible pigment dispersion can also comprise sterilant, its weight percent that accounts for the dispersion liquid gross weight is 0.0～0.2%.
3. according to the said a kind of Yellow nanometer water-type pigment dispersion of claim 1, it is characterized in that said yellow ultramarine selects the C.I. Pigment Yellow 73 74 of Switzerland vapour Bagong department (Ciba) for use.
4. according to the said a kind of Yellow nanometer water-type pigment dispersion of claim 1, it is characterized in that said polymer block polymer type dispersion agent selects the SOLsperse 43000 of U.S. Lubrizol Corp. (Lubrizol) for use.
5. according to the said a kind of Yellow nanometer water-type pigment dispersion of claim 1, it is characterized in that said wetting Agent for Printing Inks is preferred 1,2-propylene glycol, 1, ammediol, 1,4-butyleneglycol, 1,2-pentanediol, 1, the combination of one or more in the 5-pentanediol.
6. according to the said a kind of Yellow nanometer water-type pigment dispersion of claim 2, it is characterized in that said sterilant is 1, the 2-benzisothiazole-3-ketone is selected the Nipacide BIT-20 of Clariant company (Clariant) for use.
7. the preparation method of a Yellow nanometer water-type pigment dispersion 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 liquid, wetting Agent for Printing Inks and deionized water are mixed in the container according to aforementioned proportion, and stir;
2. add yellow ultramarine 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 10～20 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, preferred 1.0～3.0 hours;
6. in the process of lapping, adopted the 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% and surplus deionized water are made 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.
8. according to the preparation method of the said a kind of Yellow nanometer water-type pigment dispersion of claim 7, it is characterized in that said step 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 yellow ultramarine than macroparticle, but its effect of overlong time is no longer remarkable, so preferred 1.0～2.0 hours of shear time; Said step 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, mean diameter is between 0.05～1.00mm, and preferred rotating speed is pin bar type shredder and the zirconium oxide bead of diameter between 0.05～0.20mm of 600～4000rpm; The discharge port temperature of said step in 5. is controlled between 20～40 ℃; 6. said step is the pigment granularity Detection.
9. the preparation method of said a kind of Yellow nanometer water-type pigment dispersion according to Claim 8 is characterized in that the step of the pigment granularity Detection during said step is 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.
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| CN 200810154435 CN101597443A (en) | 2008-12-25 | 2008-12-25 | A kind of Yellow nanometer water-type pigment dispersion |
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| CN 200810154435 CN101597443A (en) | 2008-12-25 | 2008-12-25 | A kind of Yellow nanometer water-type pigment dispersion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483915A (en) * | 2013-09-11 | 2014-01-01 | 吴江市冰心文教用品有限公司 | Preparation method of pigment yellow 17 emulsion |
| CN107254194A (en) * | 2017-05-31 | 2017-10-17 | 湖北昇昊色彩科技有限公司 | The composition of paratonere 170 and its production technology |
-
2008
- 2008-12-25 CN CN 200810154435 patent/CN101597443A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103483915A (en) * | 2013-09-11 | 2014-01-01 | 吴江市冰心文教用品有限公司 | Preparation method of pigment yellow 17 emulsion |
| CN103483915B (en) * | 2013-09-11 | 2015-01-21 | 吴江华诚复合材料科技有限公司 | Preparation method of pigment yellow 17 emulsion |
| CN107254194A (en) * | 2017-05-31 | 2017-10-17 | 湖北昇昊色彩科技有限公司 | The composition of paratonere 170 and its production technology |
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Open date: 20091209 |