CN112552746A - Water-based pigment color paste and preparation method thereof - Google Patents
Water-based pigment color paste and preparation method thereof Download PDFInfo
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- CN112552746A CN112552746A CN202011371000.4A CN202011371000A CN112552746A CN 112552746 A CN112552746 A CN 112552746A CN 202011371000 A CN202011371000 A CN 202011371000A CN 112552746 A CN112552746 A CN 112552746A
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- 239000000049 pigment Substances 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 52
- 239000012860 organic pigment Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 16
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 15
- 239000011258 core-shell material Substances 0.000 claims abstract description 14
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims abstract description 10
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920005792 styrene-acrylic resin Polymers 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims description 39
- 239000006185 dispersion Substances 0.000 claims description 30
- 239000007788 liquid Substances 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 13
- 125000000129 anionic group Chemical group 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 7
- 230000000844 anti-bacterial effect Effects 0.000 claims description 6
- 239000003899 bactericide agent Substances 0.000 claims description 6
- 230000009477 glass transition Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 239000002518 antifoaming agent Substances 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 229920001228 polyisocyanate Polymers 0.000 claims description 4
- 239000005056 polyisocyanate Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 125000003342 alkenyl group Chemical group 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000001257 hydrogen Chemical group 0.000 claims description 2
- 229910052739 hydrogen Chemical group 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 12
- 239000000976 ink Substances 0.000 description 26
- 238000007639 printing Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 8
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007641 inkjet printing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000013112 stability test Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 102220032811 rs367543159 Human genes 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical group CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- NRCMAYZCPIVABH-UHFFFAOYSA-N Quinacridone Chemical compound N1C2=CC=CC=C2C(=O)C2=C1C=C1C(=O)C3=CC=CC=C3NC1=C2 NRCMAYZCPIVABH-UHFFFAOYSA-N 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- ZUQAPLKKNAQJAU-UHFFFAOYSA-N acetylenediol Chemical compound OC#CO ZUQAPLKKNAQJAU-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 1
- MYONAGGJKCJOBT-UHFFFAOYSA-N benzimidazol-2-one Chemical compound C1=CC=CC2=NC(=O)N=C21 MYONAGGJKCJOBT-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- PPSZHCXTGRHULJ-UHFFFAOYSA-N dioxazine Chemical compound O1ON=CC=C1 PPSZHCXTGRHULJ-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- PXZQEOJJUGGUIB-UHFFFAOYSA-N isoindolin-1-one Chemical compound C1=CC=C2C(=O)NCC2=C1 PXZQEOJJUGGUIB-UHFFFAOYSA-N 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 description 1
- CSHWQDPOILHKBI-UHFFFAOYSA-N peryrene Natural products C1=CC(C2=CC=CC=3C2=C2C=CC=3)=C3C2=CC=CC3=C1 CSHWQDPOILHKBI-UHFFFAOYSA-N 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical group N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Developing Agents For Electrophotography (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to the technical field of pigment color paste, in particular to water-based pigment color paste and a preparation method thereof. The color paste contains modified toner, wherein the modified toner comprises organic pigment toner and a resin core shell, the resin core shell is obtained by copolymerizing base resin and a cross-linking agent, and the base resin is water-based styrene acrylic resin or water-based styrene maleic anhydride resin. The modified toner has redispersibility, can adsorb more dispersing agents compared with common organic pigment toner, has better hydrophilicity, dispersibility and stability, and the corresponding aqueous pigment color paste has better storage stability.
Description
Technical Field
The invention relates to the technical field of pigment color paste, in particular to water-based pigment color paste and a preparation method thereof.
Background
Pigment color paste is a main colorant in an aqueous ink system, and in the field of ink-jet printing, in order to ensure the quality and the jetting performance of ink, the particle size of pigment particles in the color paste needs to reach a nanometer level, and the color paste has a narrow particle size distribution range so as to ensure pure color light, and in addition, the color paste also needs to have better storage stability, namely, the color paste can still keep stable dispersion after being stored for a longer time. However, the nano toner has small particle size and large specific surface area, and agglomeration is still likely to occur after dispersion treatment, so that the particle size of the toner particles is uneven, and further certain influence is caused on the fluidity and dispersion stability of the color paste, so that the printing quality is reduced, and ink break and printing head blockage are caused. At present, in order to improve the performance of the aqueous pigment color paste, a plurality of dispersants are purposefully introduced to the surface of toner particles in a formula level, but the particle size of the common organic toner and the number of affinity groups in molecules are relatively fixed, so that the amount of the dispersant which can be adsorbed by the toner particles has a certain upper limit, and the storage stability of the color paste cannot be ensured by simply adopting the measures.
Disclosure of Invention
The first purpose of the present invention is to provide an aqueous pigment paste using a modified toner and having good storage stability.
The second purpose of the invention is to provide a preparation method of the water-based pigment color paste.
In order to achieve the first purpose, the invention provides an aqueous pigment color paste, which is characterized by comprising modified toner, wherein the modified toner comprises organic pigment toner and a resin core shell, the resin core shell is obtained by copolymerizing base resin and a crosslinking agent, and the molecular formula of the base resin is as follows:
wherein R1 is methyl or hydrogen, and R2 is alkyl or alkenyl.
According to the scheme, the number of the affinity groups contained in the base resin which is in accordance with the molecular formula is far more than that of the affinity groups contained in the organic pigment toner particles under the same weight, so that the surface of the core-shell structure modified toner particles formed by using the resin as the master batch and performing surface modification on the organic pigment toner particles has more anchor points. And compared with other resins in the field of ink and color paste, the base resin has better hydrophilicity, and the corresponding modified toner also has redispersibility. Therefore, compared with common organic pigment toner, the modified toner can adsorb more dispersing agents, and the toner particles have better hydrophilicity, dispersibility and stability after being applied to color paste, are not easy to agglomerate even if being stored for a long time, and can obviously improve the storage stability of the color paste.
The organic pigment toner in the modified toner can be phthalocyanine, azo, quinacridone, dioxazine, isoindolinone, benzimidazolone, pyrrolidone, quinophthalone or fused ring perylene pigment toner, and the water-soluble organic solvent can be glycerol, ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, diethylene glycol monomethyl ether, propylene glycol or pyrrolidone.
Further, the acid value of the base resin is 100 or more, and the glass transition temperature of the base resin is 50 ℃ or more.
From the above, it can be seen that the resin core shell composed of the base resin satisfying the above acid value conditions can improve the dispersibility of the modified toner. The affinity group in the base resin has stronger activity under the temperature condition near Tg (glass transition temperature), so the base resin needs to be heated to be near the Tg value in the grinding preparation process of the modified toner, the Tg above 50 ℃ is obviously higher than the working temperature of room temperature and ink-jet printing ink, and the storage stability and the jetting performance of the color paste are favorably improved.
The further scheme is that the base resin is water-based styrene acrylic resin or water-based styrene maleic anhydride resin, and the cross-linking agent is polyisocyanate cross-linking agent.
Therefore, the styrene acrylic resin and the styrene maleic anhydride resin have good light transmittance, the corresponding resin core shell hardly influences color development of the toner, the two types of resin in unit weight contain more hydrophilic groups, and the corresponding resin core shell can obviously improve the dispersibility and the storage stability of the organic pigment toner.
At present, in mainstream manufacturers, there are types satisfying the requirements of the acid value and the Tg value in HIROS series aqueous styrene acrylic resin of Nippon starlight PMC corporation and XIRAN series aqueous styrene maleic anhydride resin of PolySCOPE corporation in the Netherlands.
The further proposal is that the water-based pigment color paste comprises 10 to 30 percent of modified toner, 5 to 10 percent of water-soluble organic solvent, 3 to 5 percent of anionic dispersant, 0.5 to 2 percent of auxiliary agent composition and the balance of water according to weight percentage. The auxiliary composition comprises a pH regulator, a defoaming agent and a bactericide.
Therefore, the modified toner and the anionic dispersant which accord with the proportion relationship can be stably adsorbed and combined, and the pigment color paste which accords with the proportion has a stable dispersion system and good storage stability.
Further, the anionic dispersant is selected from BYK 190 and BYK 192 of Bikk, Germany, ZetaSperse 3100 and ZetaSperse 3700 of gas chemistry, or two of them.
Therefore, the anionic dispersant and the base resin are stably combined through Van der Waals force and the attractive force between ions, and meanwhile, the chain segment of the dispersant extends in the solvent, so that a dispersion position resistance layer with the thickness of more than 100A can be formed on the surface of the modified toner particles, the modified toner particles can be effectively prevented from agglomerating, and the filtering performance cannot be influenced by the viscosity of the color paste.
It should be noted that, the color paste formula is specific, each component has a plurality of specific substances to be selected, the specific substances corresponding to the same component are relatively close in physical and chemical properties, the reaction hardly occurs, and the deterioration of the related performance of the color paste is not caused after the color paste formula is mixed, so that the specific implementation can be realized by mixing the substances serving as the same component according to the needs.
The further proposal is that the viscosity of the aqueous pigment color paste is 2cP to 10cP, the surface tension is 35mN/m to 70mN/m, and the average particle diameter is 100nm to 130 nm.
Therefore, the aqueous pigment color paste with lower viscosity is suitable for preparing low-viscosity ink, the ink corresponding to the color paste with higher surface tension can better adapt to high-speed printing, and the color paste with smaller average particle size is not easy to cause end blockage.
In order to achieve the second object, the invention provides a preparation method of the aqueous pigment paste, which is characterized by comprising the following steps:
s1: stirring and mixing 30 to 50 weight percent of organic pigment toner, 5 to 10 weight percent of base resin, 1 to 4 weight percent of cross-linking agent and the balance of aqueous organic solvent at room temperature at the rotating speed of 800rpm to 1200rpm for 30 to 60min to obtain a first dispersion liquid.
S2: grinding the first dispersion liquid for 2 to 3 hours under the conditions of the glass transition temperature of the base resin +/-5 ℃ and the rotating speed of 2000rpm to 2500rpm, filtering the ground first dispersion liquid by using a filter membrane with the aperture of 0.45 mu m, drying the filtrate by distillation, crushing the dried filtrate, and sieving the dried filtrate by using a 500-mesh sieve to obtain the modified toner.
S3: 10 to 30 percent of modified toner, 5 to 10 percent of aqueous organic solvent, 3 to 5 percent of anionic dispersant, 0.5 to 2 percent of auxiliary agent composition and the balance of water are stirred and mixed for 1 to 2 hours at room temperature at the rotating speed of 800rpm to 1200rpm to obtain a second dispersion liquid.
S4: grinding the second dispersion liquid at room temperature and at the rotating speed of 1500 rpm-2000 rpm for 4 h-6 h, centrifuging at the rotating speed of 6000 rpm-8000 rpm for 10 min-20 min, filtering with a filter membrane with the aperture of 1.0 μm, and taking the filtrate.
According to the scheme, the step S2 can ensure that the resin base resin and the cross-linking agent are fully cross-linked and coated on the surfaces of the organic pigment toner particles to form the modified toner with the core-shell structure under the appropriate temperature condition, rotation speed condition and grinding time length. Step S4 can ensure that the modified toner fully absorbs the anionic dispersant and forms a stable dispersion system with other components through long-time grinding treatment, and color paste with uniform particle size and ideal average particle size can be obtained after centrifugation and filtration treatment.
It should be noted that, the raw materials related to the above preparation method are all aqueous solutions or aqueous dispersions except the organic pigment toner and the modified toner, and the corresponding commercially available products have relatively fixed solid contents, and color paste manufacturers generally do not perform concentration or dilution treatment before use. Specifically, the solid content ranges of the commercially available water-based styrene acrylic resin, the water-based styrene maleic anhydride resin and the cross-linking agent are generally 30 wt% to 40 wt%, so that the weight ratio of the corresponding liquid commercially available product is substantially consistent with the weight ratio of the actual solid content, and the ratio range of the resin core-shell thickness to the toner particle size of the core-shell structure modified toner prepared by using the fixed organic pigment toner and the base resin under the same process conditions is relatively fixed.
In a further scheme, the filtrate is dried by distillation at the temperature of 80-100 ℃ in the step S2.
Therefore, the modified toner can be effectively protected by evaporating the filtrate at a lower temperature, and the resin core shell is prevented from being thermally denatured or melted and adhered.
Further, the first dispersion or the second dispersion is subjected to the milling treatment in steps S2 and S4 using a mill having a zirconium bead loading of 70% to 80% and a zirconium bead particle size of 0.3 mm.
Therefore, the grinding machine which adopts the zirconium beads with the particle size specification and the filling amount meeting the requirements can achieve a better grinding effect on the first dispersion liquid and the second dispersion liquid, so that the average particle size of the finished color paste is controlled within an ideal range.
Detailed Description
The invention prepares the water-based pigment color paste according to the following steps:
s1: according to the weight percentage, 30 to 50 percent of organic pigment toner, 5 to 10 percent of base resin, 1 to 4 percent of cross-linking agent and the balance of aqueous organic solvent are stirred and mixed for 30 to 60 minutes at room temperature at the rotating speed of 800rpm to 1200rpm to obtain first dispersion liquid, wherein the base resin is aqueous styrene acrylic resin or aqueous styrene maleic anhydride resin, and the cross-linking agent is polyisocyanate cross-linking agent.
S2: grinding the first dispersion liquid for 2h to 3h by using a horizontal grinding machine under the conditions of the glass transition temperature of the base resin being +/-5 ℃ and the rotating speed of 2000rpm to 2500rpm, filtering by using a filter membrane with the aperture of 0.45 mu m, using zirconium beads with the particle size of 0.3mm by using the horizontal grinding machine, wherein the filling amount of the zirconium beads is 70% to 80%, drying the filtrate by evaporation at the temperature of 80 ℃ to 100 ℃, putting the dried filtrate into a pigment grinder for grinding, and sieving by using a 500-mesh sieve to obtain the modified toner.
S3: 10 to 30 percent of modified toner, 5 to 10 percent of aqueous organic solvent, 3 to 5 percent of anionic dispersant, 0.5 to 2 percent of auxiliary agent composition and the balance of water are stirred and mixed for 1 to 2 hours at room temperature at the rotating speed of 800rpm to 1200rpm to obtain a second dispersion liquid according to the weight percentage, wherein the auxiliary agent composition comprises a pH regulator, an antifoaming agent and a bactericide.
S4: and grinding the second dispersion solution for 4 to 6 hours by using a horizontal grinding machine under the conditions of room temperature and the rotating speed of 1500 to 2000rpm, wherein the horizontal grinding machine uses zirconium beads with the particle size of 0.3mm and the filling amount of the zirconium beads is 70 to 80 percent, then centrifuging for 10 to 20 minutes under the rotating speed of 6000 to 8000rpm, and finally filtering by using a filter membrane with the aperture of 1.0 mu m to obtain the aqueous pigment color paste.
Examples one to four
In the first to the fourth embodiments, the aqueous pigment color paste is prepared according to the above method, and the specific component ratios of the related modified toner and color paste are shown in tables 1 and 2. BG-NIP PV FAST BLUE (cyan), INK jet MAGENTA E02 (MAGENTA), INK jet Yellow 4GC (Yellow) and PALIOT Black L0080 (Black) from BASF of Crayne were used as organic pigment toners in the examples; HIROS X-1 aqueous phenylacetic acid acrylic resin of Japanese star light PMC and XIRAN 1000H aqueous styrene maleic anhydride resin of PolySCOPE of Netherlands are used as base resins, the acid value of both base resins is above 100, and Tg is above 50 ℃.
In addition, as the polyisocyanate crosslinking agent, IT AD201D by JETIC corporation; the anionic dispersant is BYK 190 and BYK 192 of Bike Germany and ZetaSperse 3100 and ZetaSperse 3700 of American gas chemistry; the water-soluble organic solvent used was propylene glycol, the pH adjusting agent used was triethanolamine, the antifoaming agent used was BYK-094 available from Bike, Germany, and the bactericide used was MERGAL K10N available from TROY.
Table 1: modified toner ingredient list
Table 2: ingredient list of water-based pigment color paste
The modified toner prepared from the groups A to D and 5g of the corresponding organic pigment toner are respectively sprinkled into 8 beakers filled with 100ml of deionized water, the beakers are stirred by a glass rod and then stand still, the dispersion state is observed, the four organic pigment toner particles are in an agglomerated state after being dispersed in the water, and the four modified toner particles can be kept in the dispersed state all the time, which shows that the surfaces of the toner particles can have certain hydrophilicity and are not easy to agglomerate after surface modification by the method, so that the expected modification purpose is achieved.
The viscosity of the aqueous pigment color paste prepared by the first to the fourth examples is 2cP to 10cP, the surface tension is 35mN/m to 70mN/m, and the average particle size is 100nm to 130 nm.
Ink color Density test
The four-color water-based pigment color paste prepared in the first to fourth embodiments and the four-color water-based pigment color paste finished product of the main stream manufacturer in the market are respectively prepared into the water-based pigment ink according to the same method, and the preparation method of the water-based pigment ink is as follows:
30 percent of pigment color paste, 10 percent of acrylic resin, 1.0 percent of alkynediol surfactant, 0.1 percent of bactericide and the balance of water are taken according to the weight percentage, stirred and mixed for 60min at the room temperature at the rotating speed of 1000rpm, and then filtered by a filter membrane with the aperture of 0.45 mu m. Wherein the acrylic resin is NeoCryl BT-107-S from Dismann, the acetylenediol surfactant is Surfynol 465 from American gas chemical, and the bactericide is MERGAL K10N from TROY.
The ink is taken and used for printing a single color block on white pure cotton cloth by a black P-PRESS digital direct injection printing machine according to 100% ink jet setting, and then an X-RITE 528 color measuring instrument is used for carrying out color density test on the printed color block, and the test result is shown in a table 3. In Table 3, the inks used in the comparative examples were prepared from commercially available mill bases, and the same color mill bases were used in the same numbered examples and comparative examples to prepare the inks. As can be seen from Table 3, the inks prepared using the pastes of examples one to four were very similar in both L value (representing black and white, "+" representing white, and "-" representing dark), a value (representing red and green, "+" representing red, and "-" representing green) and b value (representing yellow and blue, "+" representing yellow and "-" representing blue) to the inks prepared from the commercial paste products, and thus were substantially identical in color development.
Table 3: color Density test results
Ink printing fluency test
500ml of each of the aqueous pigment inks corresponding to the first to fourth examples in the "ink color density test" was taken, and the ink was continuously printed with an EPSON 4720 printer according to a single color block and 100% inkjet setting while observing, and the printing medium was paper.
The observation shows that the water-based pigment ink corresponding to the first to fourth examples can be used for continuously printing 500ml, and the printing is smooth and has no white line, so that the water-based pigment ink prepared by the invention has good jetting performance, and can be used for preparing ink-jet printing ink.
Color paste storage stability test
The aqueous pigment color pastes prepared in the first to fourth examples and the commercially available color pastes used in the ink color density test were aged in a thermostat at 60 ℃ for four weeks, each color paste was tested for pH, conductivity, surface tension, viscosity and particle size before and after the aging treatment and the corresponding change rate was calculated, and the color paste was judged to be acceptable if the change rate was less than 5%, and the test results are shown in Table 4. The D50 value in Table 4 represents the particle size corresponding to a cumulative percent particle size distribution of 50%, i.e., particles having a particle size greater than this value account for 50% and particles less than this value account for 50%, and the definition of the D90 value follows a similar logic. In table 4, the change rate is calculated by dividing the absolute value of the difference between the detection values in the detection items before and after aging by the detection value of the corresponding detection item before aging. As can be seen from Table 4, the color pastes corresponding to the first to fourth examples are all qualified in the storage stability test under the detection items of pH value, conductivity, surface tension, viscosity and particle size, and the change rate under most detection items is superior to that of the commercially available color paste, which indicates that the aqueous pigment color paste prepared by the invention has better storage stability.
Table 4: storage stability test results
Claims (9)
1. The water-based pigment color paste is characterized by comprising the following components in parts by weight:
the modified toner comprises an organic pigment toner and a resin core shell, wherein the resin core shell is obtained by copolymerizing a base resin and a crosslinking agent, and the molecular formula of the base resin is as follows:
wherein R1 is methyl or hydrogen, and R2 is alkyl or alkenyl.
2. The aqueous pigment paste according to claim 1, wherein:
the acid value of the base resin is 100 or more, and the glass transition temperature of the base resin is 50 ℃ or more.
3. The aqueous pigment paste according to claim 1, wherein:
the base resin is water-based styrene acrylic resin or water-based styrene maleic anhydride resin, and the cross-linking agent is a polyisocyanate cross-linking agent.
4. The aqueous pigment paste according to any one of claims 1 to 3, wherein:
the toner comprises, by weight, 10% to 30% of modified toner, 5% to 10% of water-soluble organic solvent, 3% to 5% of anionic dispersant, 0.5% to 2% of an auxiliary composition and the balance of water, wherein the auxiliary composition comprises a pH regulator, an antifoaming agent and a bactericide.
5. The aqueous pigment paste according to claim 4, wherein:
the anionic dispersant is selected from one or two of BYK 190, BYK 192, ZetaSperse 3100 and ZetaSperse 3700.
6. The aqueous pigment paste according to claim 4, wherein:
the viscosity of the aqueous pigment color paste is 2cP to 10cP, the surface tension is 35mN/m to 70mN/m, and the average particle size is 100nm to 130 nm.
7. The process for preparing an aqueous pigment paste according to any one of claims 4 to 6 comprising the steps of:
s1: stirring and mixing 30 to 50 weight percent of organic pigment toner, 5 to 10 weight percent of base resin, 1 to 4 weight percent of cross-linking agent and the balance of aqueous organic solvent at room temperature at the rotating speed of 800rpm to 1200rpm for 30 to 60min to obtain a first dispersion liquid;
s2: grinding the first dispersion liquid for 2 to 3 hours under the conditions of the glass transition temperature of the base resin being +/-5 ℃ and the rotating speed of 2000rpm to 2500rpm, filtering the ground first dispersion liquid by using a filter membrane with the aperture of 0.45 mu m, drying the filtrate by distillation, crushing the dried filtrate, and sieving the dried filtrate by using a 500-mesh sieve to obtain modified toner;
s3: stirring and mixing 10 to 30 percent of modified toner, 5 to 10 percent of aqueous organic solvent, 3 to 5 percent of anionic dispersant, 0.5 to 2 percent of auxiliary agent composition and the balance of water at room temperature at the rotating speed of 800rpm to 1200rpm for 1 to 2 hours to obtain a second dispersion liquid according to the weight percentage;
s4: and grinding the second dispersion liquid at room temperature and at the rotating speed of 1500rpm to 2000rpm for 4h to 6h, centrifuging the second dispersion liquid at the rotating speed of 6000rpm to 8000rpm for 10min to 20min, and filtering the second dispersion liquid through a filter membrane with the aperture of 1.0 mu m to obtain filtrate.
8. The preparation method of the water-based pigment paste according to claim 7, wherein the method comprises the following steps:
in step S2, the filtrate is dried by distillation at 80-100 ℃.
9. The preparation method of the water-based pigment paste according to claim 7, wherein the method comprises the following steps:
the first dispersion or the second dispersion is subjected to grinding treatment in steps S2 and S4 using a grinder with a zirconium bead loading of 70% to 80% and a zirconium bead particle size of 0.3 mm.
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| CN202011371000.4A CN112552746A (en) | 2020-11-30 | 2020-11-30 | Water-based pigment color paste and preparation method thereof |
| PCT/CN2021/134029 WO2022111689A1 (en) | 2020-11-30 | 2021-11-29 | Water-based pigment colour paste and preparation method therefor |
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| WO2022111689A1 (en) * | 2020-11-30 | 2022-06-02 | 珠海天威新材料股份有限公司 | Water-based pigment colour paste and preparation method therefor |
| CN114736533A (en) * | 2022-04-13 | 2022-07-12 | 苏州世名科技股份有限公司 | Surface modified organic pigment, modification method and application thereof, and color master batch containing surface modified organic pigment |
| CN116376314A (en) * | 2023-04-13 | 2023-07-04 | 宇虹颜料股份有限公司 | Preparation method of pigment with high tinting strength and high transparency in aqueous application |
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