WO2022111689A1 - 一种水性颜料色浆及其制备方法 - Google Patents
一种水性颜料色浆及其制备方法 Download PDFInfo
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- WO2022111689A1 WO2022111689A1 PCT/CN2021/134029 CN2021134029W WO2022111689A1 WO 2022111689 A1 WO2022111689 A1 WO 2022111689A1 CN 2021134029 W CN2021134029 W CN 2021134029W WO 2022111689 A1 WO2022111689 A1 WO 2022111689A1
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- Prior art keywords
- water
- based pigment
- pigment paste
- toner
- resin
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 239000000049 pigment Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 54
- 229920005989 resin Polymers 0.000 claims abstract description 54
- 239000012860 organic pigment Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 16
- 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 41
- 239000006185 dispersion Substances 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- 125000000129 anionic group Chemical group 0.000 claims description 12
- 239000011258 core-shell material Substances 0.000 claims description 12
- 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
- 239000000706 filtrate Substances 0.000 claims description 8
- 230000009477 glass transition Effects 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000011148 porous material 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
- 239000002253 acid Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 5
- 239000005056 polyisocyanate Substances 0.000 claims description 5
- 229920001228 polyisocyanate Polymers 0.000 claims description 5
- 239000002671 adjuvant Substances 0.000 claims description 3
- 239000002518 antifoaming agent Substances 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 239000003002 pH adjusting agent Substances 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
- 239000012528 membrane Substances 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 16
- 239000000976 ink Substances 0.000 description 25
- 239000003086 colorant Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000007639 printing Methods 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 5
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 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
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 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 compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- LHYQAEFVHIZFLR-UHFFFAOYSA-L 4-(4-diazonio-3-methoxyphenyl)-2-methoxybenzenediazonium;dichloride Chemical compound [Cl-].[Cl-].C1=C([N+]#N)C(OC)=CC(C=2C=C(OC)C([N+]#N)=CC=2)=C1 LHYQAEFVHIZFLR-UHFFFAOYSA-L 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
- 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
- 238000004040 coloring Methods 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000013530 defoamer Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- PPSZHCXTGRHULJ-UHFFFAOYSA-N dioxazine Chemical compound O1ON=CC=C1 PPSZHCXTGRHULJ-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 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
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005374 membrane filtration Methods 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
- -1 quinophthalone Ketone Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002002 slurry 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
Definitions
- the invention is based on the Chinese patent with the patent number of 202011371000.4 and the title of "a water-based pigment paste and its preparation method".
- the invention relates to the field of pigment paste, in particular to a water-based pigment paste and a preparation method thereof.
- Pigment paste is the main colorant in the water-based ink system.
- the particle size of the pigment particles in the color paste In the field of inkjet printing, in order to ensure the quality of the ink and its jetting performance, the particle size of the pigment particles in the color paste must reach the nanometer level and have a narrow particle size.
- the distribution range is to ensure the purity of the shade, and it also needs to have good storage stability, that is, to ensure that the color paste can remain stable and dispersed after a long time of storage.
- agglomeration may still occur after the dispersion treatment, which makes the particle size of the toner particles uneven, which in turn has a certain impact on the fluidity and dispersion stability of the color paste.
- the first object of the present invention is to provide a water-based pigment paste with good storage stability using modified toner.
- the second object of the present invention is to provide a preparation method of the above water-based pigment paste.
- the present invention provides a water-based pigment paste, which is special in that it includes a modified toner, and the modified toner includes an organic pigment toner and a resin core-shell, and the resin core-shell is composed of a base resin and a resin.
- the cross-linking agent is copolymerized to obtain, and the molecular formula of the base resin is:
- R1 is methyl or hydrogen
- R2 is alkyl or alkenyl
- the organic pigment toner in the above-mentioned modified toner can be phthalocyanine, azo, quinacridone, dioxazine, isoindolinone, benzimidazolone, pyrrolidone, quinophthalone Ketone or fused ring perylene pigment toner, water-soluble organic solvent can be selected from glycerol, ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, diethylene glycol methyl ether, propylene glycol or pyrrolidone.
- a further solution is that the acid value of the base resin is above 100, and the glass transition temperature of the base resin is above 50°C.
- the base resin is a water-based styrene acrylic resin or a water-based styrene maleic anhydride resin
- the cross-linking agent is a polyisocyanate cross-linking agent
- the base resin that meets the above requirements of acid value and Tg value can be selected from the HIROS series of water-based styrene acrylic resins from Japan Starlight PMC Co., Ltd. and the XIRAN series of water-based styrene maleic anhydride resins from the Netherlands POLYSCOPE Company.
- the water-based pigment paste comprises 10% to 30% of modified toner, 5% to 10% of water-soluble organic solvent, 3% to 5% of anionic dispersant, 0.5% to 5% by weight 2% of the adjuvant composition, the balance being water.
- the adjuvant composition includes pH adjusters, antifoaming agents and bactericides.
- anionic dispersant is selected from one or both of BYK 190 and BYK 192 from BYK, ZetaSperse 3100 and ZetaSperse 3700 from American Gas Chemicals.
- the above-mentioned color paste formula is specific to each component, and there are various specific substances to choose from.
- the physical and chemical properties of various specific substances corresponding to the same component are relatively close, and they hardly react with each other.
- the performance of the colorant is deteriorated, so a variety of substances of the same component can be mixed as needed in the specific implementation.
- a further solution is that the viscosity of the aqueous pigment paste is 2cP to 10cP, the surface tension is 35mN/m to 70mN/m, and the average particle size is 100nm to 130nm.
- the present invention provides a preparation method of the aforementioned water-based pigment paste, which is special in that it comprises the following steps:
- S2 grind the first dispersion liquid under the temperature condition of the glass transition temperature of the base resin ⁇ 5°C and the rotational speed of 2000rpm to 2500rpm for 2h to 3h, then filter it with a 0.45 ⁇ m pore size filter membrane, take the filtrate and evaporate it to dryness, pulverize and filter it. 500-mesh sieve to obtain modified toner.
- S3 10% to 30% of modified toner, 5% to 10% of aqueous organic solvent, 3% to 5% of anionic dispersant, 0.5% to 2% of auxiliary agent composition and The remaining water is stirred and mixed at room temperature at a rotational speed of 800 rpm to 1200 rpm for 1 h to 2 h to obtain a second dispersion.
- the second dispersion is ground at room temperature and at a rotational speed of 1500 rpm to 2000 rpm for 4 h to 6 h, centrifuged at a rotational speed of 6000 rpm to 8000 rpm for 10 min to 20 min, and filtered through a 1.0 ⁇ m pore size filter to obtain the filtrate.
- the various raw materials involved in the above preparation method are all aqueous solutions or aqueous dispersions except the organic pigment toner and the modified toner, and the solid content of the corresponding commercial products is relatively fixed, and color paste manufacturers generally do not use it before use. Concentrate or dilute.
- the solid content of commercially available water-based styrene acrylic resin, water-based styrene maleic anhydride resin and cross-linking agent is usually in the range of 30wt% to 40wt%, so the weight ratio of the corresponding liquid commercial product to the actual solid weight
- the ratios are basically the same, and the ratio of the resin core-shell thickness to the toner particle size of the core-shell modified toner prepared by using a fixed variety of organic pigment toner and base resin under the same process conditions is also relatively fixed.
- step S2 the filtrate is placed under a temperature condition of 80°C to 100°C and evaporated to dryness.
- a further solution is that in steps S2 and S4, the first dispersion liquid or the second dispersion liquid is ground and processed by using a mill with a filling amount of zirconium beads of 70% to 80% and a particle size of the zirconium beads of 0.3 mm.
- the organic pigment toner is used as the master batch.
- the core-shell structure modified toner particles formed after surface modification of the resin have more anchor points on the surface.
- the above-mentioned base resin has better hydrophilicity than other resins in the field of ink and colorant, and the corresponding modified toner also has redispersibility. Therefore, the above modified toners can absorb more dispersants than ordinary organic pigment toners, and the toner particles have better hydrophilicity, dispersibility and stability after being applied to the colorants, and it is not easy to occur even if stored for a long time. Agglomeration can significantly improve the storage stability of the colorant.
- the resin core-shell formed by the base resin meeting the condition that the acid value is above 100 can improve the dispersion performance of the modified toner.
- the affinity groups in the base resin have strong activity at the temperature near the Tg (glass transition temperature) value, so the modified toner needs to be heated to the Tg value near the base resin in the process of grinding and preparing the modified toner.
- Tg is obviously higher than room temperature and the working temperature of inkjet printing ink, which is beneficial to improve the storage stability and jetting performance of color paste.
- Styrene acrylic resin and styrene maleic anhydride resin have good light transmittance, the corresponding resin core-shell hardly affects the color development of toner, and the two types of resins contain a large number of hydrophilic groups per unit weight.
- the resin core-shell can significantly improve the dispersibility and storage stability of organic pigment toners.
- the modified toner and the anionic dispersant in the above-mentioned certain ratio can be adsorbed and combined stably, and the pigment paste that meets the above-mentioned ratio has a stable dispersion system and good storage stability.
- the specific type of anionic dispersant mentioned above is stably combined with the base resin through van der Waals force and the attractive force between ions, and the segment of the dispersant is stretched in the solvent, and a dispersion steric hindrance layer with a thickness of >100A can be formed on the surface of the modified toner particles. , which can effectively prevent the agglomeration of modified toner particles, and will not significantly change the viscosity of the colorant and affect the filtration performance.
- the lower viscosity water-based pigment paste is suitable for preparing low-viscosity ink, the ink corresponding to the higher surface tension paste can be better adapted to high-speed printing, and the color paste with a smaller average particle size is less prone to clogging.
- step S2 can ensure that the resin base resin and the cross-linking agent are fully cross-linked and coated on the surface of the organic pigment toner particles under suitable temperature conditions, rotational speed conditions and grinding time. Structured modified toner. Step S4 can ensure that the modified toner can fully absorb the anionic dispersant and form a stable dispersion system with other components through a long-time grinding treatment, and then after centrifugation and filtration treatment, a color paste with uniform particle size and an ideal average particle size can be obtained. .
- step S2 the filtrate is evaporated to dryness at a lower temperature, which can effectively protect the modified toner and prevent the resin core-shell from being denatured by heat or melting and sticking.
- step S2 and step S4 respectively adopt the zirconium beads of above-mentioned particle size specifications and the grinding machine whose filling amount meets the above-mentioned requirements can have a better grinding effect for the first dispersion liquid and the second dispersion liquid, so as to reduce the size of the finished color paste.
- the average particle size is controlled within the desired range.
- the present invention prepares water-based pigment paste according to the following steps:
- the first dispersion liquid is obtained by stirring and mixing at a rotational speed for 30 to 60 minutes.
- the base resin is a water-based styrene acrylic resin or a water-based styrene maleic anhydride resin
- the cross-linking agent is a polyisocyanate cross-linking agent.
- the first dispersion liquid is ground for 2h to 3h with a horizontal grinder under the temperature conditions of the glass transition temperature of the base resin ⁇ 5°C and the rotational speed of 2000rpm to 2500rpm, and then filtered with a 0.45 ⁇ m pore size filter.
- the horizontal grinder Use 0.3mm particle size zirconium beads and the filling amount of zirconium beads is 70% to 80%, take the filtrate and evaporate it to dryness at a temperature of 80 ° C to 100 ° C, put it into a pigment pulverizer to pulverize and pass through a 500-mesh sieve to obtain a modified toner .
- auxiliary composition includes a pH adjuster, a defoaming agent and a bactericide.
- the second dispersion is ground for 4h to 6h using a horizontal mill at room temperature and at a rotational speed of 1500rpm to 2000rpm.
- the horizontal mill uses zirconium beads with a particle size of 0.3 mm and the filling amount of the zirconium beads is 70% to 80%. %, then centrifuged for 10 to 20 minutes at a rotational speed of 6000 rpm to 8000 rpm, and finally filtered through a 1.0 ⁇ m pore size filter to obtain an aqueous pigment paste.
- Example 1 to 4 water-based pigment pastes were prepared according to the above method, and the specific composition ratios of the modified toners and pastes involved are shown in Tables 1 and 2.
- Clariant's BG-NIP PV FAST BLUE (cyan), INK jet MAGENTA E02 (magenta), INK jet Yellow 4GC (yellow) and BASF's Paliotol Black L0080 (black) were used as organic pigment toners; Japan was used Starlight PMC's HIROS X-1 water-based phenylacetic acid acrylic resin and the Netherlands POLYSCOPE XIRAN 1000H water-based styrene maleic anhydride resin are used as the base resins.
- the polyisocyanate crosslinking agent uses IT AD201D of JETIC company; the anionic dispersant uses BYK 190, BYK 192 from BYK and ZetaSperse 3100 and ZetaSperse 3700 from American Gas Chemical; the water-soluble organic solvent uses propylene glycol, and the pH adjuster is used Triethanolamine, BYK-094 from BYK, Germany is used as defoamer, and MERGAL K10N from TROY is used as bactericide.
- the viscosity of the water-based pigment paste prepared in Examples 1 to 4 is all 2cP to 10cP, the surface tension is all 35mN/m to 70mN/m, and the average particle size is all 100nm to 130nm.
- acrylic resin selects NeoCryl BT-107-S of Dutch DSM for use
- acetylenic diol surfactant selects Surfynol 465 of American Gas Chemicals for use
- bactericide uses MERGAL K10N of TROY Company.
- the inks prepared by using the colorants of Examples 1 to 4 and the inks prepared by commercially available colorants are in the L value (characterizing black and white, "+” means white, “-” means dark), a Values (representing red and green, “+” means reddish, “-” means greenish) and b value (representing yellow and blue, "+” means yellowish, “-” means blueish) are very close, so in the display
- L value characterizing black and white, "+” means white, "-” means dark
- a Values (representing red and green, "+” means reddish, "-” means greenish)
- b value respectively representing yellow and blue, "+” means yellowish, "-” means blueish
- the water-based pigment inks corresponding to Examples 1 to 4 can print 500ml continuously, and the printing is smooth without white lines, which proves that the water-based pigment inks corresponding to the water-based pigment pastes prepared by the present invention have good jetting performance.
- the slurry can be used to prepare inkjet printing inks.
- the water-based pigment pastes prepared in Examples 1 to 4 and the commercially available color pastes used in the "ink color density test" were placed in a 60°C incubator for four weeks of aging, and each color paste was tested for pH value and electrical conductivity before and after the aging treatment. , surface tension, viscosity and particle size and calculate the corresponding change rate, the change rate is less than 5% can be judged as qualified, the test results are shown in Table 4.
- the D50 value in Table 4 represents the corresponding particle size when the cumulative particle size distribution percentage reaches 50%, that is, the particles with a particle size larger than this value account for 50%, and the particles smaller than it also account for 50%.
- the definition of the D90 value also follows a similar logic. .
- the absolute value of the difference between the detection values of each detection item before and after aging is divided by the detection value of the corresponding detection item before aging.
- the storage stability tests of the colorants corresponding to Examples 1 to 4 are all qualified in the pH value, electrical conductivity, surface tension, viscosity and particle size testing items, and the changes in most testing items The ratios are better than those of the commercially available color paste, indicating that the water-based pigment paste prepared by the present invention has better storage stability.
- the invention is used to prepare the water-based pigment paste with better storage stability, and make the water-based pigment paste have better hydrophilicity, dispersibility and stability.
- the color powder selected in the water-based pigment paste of the present invention has good dispersibility, and the core-shell structure modified toner particles formed by the modified basic tree, so that the surface has more anchor points, so that the color powder can be It is not easy to agglomerate when stored for a long time, thereby improving the storage stability of the colorant.
- the base resin, polyisocyanate crosslinking agent, and anionic dispersant with an acid value above 100 and a glass transition temperature above 50 °C, and controlling the dosage of each component of the water-based pigment paste, the viscosity, The surface tension and average particle size are controlled within a certain range, and then by controlling the appropriate temperature, rotation speed, grinding time and other preparation conditions when preparing the color paste, the prepared color paste has a stable dispersion system and good storage stability.
- the water-based pigment paste of the present invention is widely used in the coloring of the water-based ink system to ensure the quality of the ink and its jetting performance.
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- 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
本发明涉及颜料色浆技术领域，并本发明提供一种水性颜料色浆及其制备方法，具体是一种水性颜料色浆及其制备方法。该色浆含有改性色粉，改性色粉包括有机颜料色粉和树脂核壳，树脂核壳由基础树脂与交联剂共聚得到，基础树脂为水性苯乙烯丙烯酸树脂或水性苯乙烯马来酸酐树脂。上述改性色粉具备再分散性，相比普通有机颜料色粉能够吸附更多分散剂，且具备更好的亲水性、分散性和稳定性，对应的水性颜料色浆具备较好的储存稳定性。
Description
本发明基于专利号为202011371000.4、名称为“一种水性颜料色浆及其制备方法”的中国专利，本发明涉及颜料色浆领域，尤其是涉及一种水性颜料色浆及其制备方法。
颜料色浆是水性墨水体系中主要的着色剂，而在喷墨打印领域，为保证墨水的品质及其喷射性能，色浆中颜料颗粒的粒径须达到纳米级别，并且具备较窄的粒径分布范围以保证色光纯正，另外还需具备较好的储存稳定性，即保证色浆在储存较长时间后仍能保持稳定分散。但是由于纳米色粉的粒径小，比表面积较大，经分散处理后仍有可能发生团聚，使色粉颗粒粒径不均，进而对色浆的流动性和分散稳定性造成一定的影响，导致打印质量降低，造成断墨和打印头堵塞。目前为改善水性颜料色浆的上述性能通常会在配方层面针对性地引入多种分散剂吸附到色粉粒子表面，但常用的有机色粉的粒径和分子中的亲和基团数均较为固定，因此色粉粒子可吸附分散剂的量存在一定上限，单纯采取上述手段仍不足以保证色浆的储存稳定性。
本发明的第一目的在于提供一种使用改性色粉且具备良好储存稳定性的水性颜料色浆。
本发明的第二目的在于提供一种上述水性颜料色浆的制备方法。
为实现上述第一目的，本发明提供一种水性颜料色浆，其特殊之处在于，包括改性色粉，改性色粉包括有机颜料色粉和树脂核壳，树脂核壳由基础树脂与交联剂共聚得到，基础树脂的分子式为：
其中，R1为甲基或氢，R2为烷基或烯基。
上述改性色粉中有机颜料色粉可以是酞菁类，偶氮类，喹吖碇酮类，二噁嗪类，异吲哚啉酮类、苯骈咪唑酮类、吡咯酮类、喹酞酮类或稠环苝系颜料色粉，水溶性有机溶剂可选用丙三醇、乙二醇、二甘醇、三甘醇、聚乙二醇、二乙二醇甲醚、丙二醇或吡咯烷酮。
进一步的方案是，基础树脂的酸值在100以上，基础树脂的玻璃化温度在50℃以上。
进一步的方案是，基础树脂为水性苯乙烯丙烯酸树脂或水性苯乙烯马来酸酐树脂，交联剂为多异氰酸酯交联剂。
符合上述酸值及Tg值要求的基础树脂可选用目前在主流厂商中的日本星光PMC株式会社的HIROS系列水性苯乙烯丙烯酸树脂，以及荷兰POLYSCOPE公司的XIRAN系列水性苯乙烯马来酸酐树脂。
进一步的方案是，水性颜料色浆按重量百分比计包括10％至30％的改性色粉、5％至10％的水溶性有机溶剂、3％至5％的阴离子型分散剂、0.5％至2％的助剂组合物，余量为水。助剂组合物包括pH调节剂、消泡剂和杀菌剂。
进一步的方案是，阴离子型分散剂选自德国毕克的BYK 190、BYK 192、美国气体化学的ZetaSperse 3100、ZetaSperse 3700中的一种或两种。
上述色浆配方具体到每个成分都存在多种具体的物质可供选择，对应于同一成分的多种具体物质在物化性质上都较为接近，相互间几乎不发生反应，混用后也不会造成色浆相关性能的劣化，因此具体实施时可根据需要混用作为同一成分的多种物质。
进一步的方案是，水性颜料色浆的粘度为2cP至10cP，表面张力为35mN/m至70mN/m，平均粒径为100nm至130nm。
为实现上述第二目的，本发明提供一种前述水性颜料色浆的制备方法，其特殊之处在于，包括下列步骤：
S1：按重量百分比计将30％至50％的有机颜料色粉、5％至10％的基础树脂、1％至4％的交联剂和余量水性有机溶剂在室温下以800rpm至1200rpm的转速搅拌混合30min至60min得到第一分散液。
S2：将第一分散液在基础树脂的玻璃化温度±5℃的温度条件及2000rpm至2500rpm的转速条件下研磨处理2h至3h后用0.45μm孔径滤膜过滤，取滤液蒸干后粉碎并过500目筛得到改性色粉。
S3：按重量百分比计将10％至30％的改性色粉、5％至10％的水性有机溶剂、3％至5％的阴离子型分散剂、0.5％至2％的助剂组合物以及余量水在室温下以800rpm至1200rpm的转速搅拌混合1h至2h得到第二分散液。
S4：将第二分散液在室温及1500rpm至2000rpm的转速条件下研磨处理4h至6h后在6000rpm至8000rpm的转速条件下离心10min至20min，再经1.0μm孔径滤膜过滤后取滤液。
上述制备方法涉及的各种原料除有机颜料色粉和改性色粉外均为水溶液或水性分散液，且对应的市售品固含量均较为固定，色浆生产商在使用前一般也不会做浓缩或稀释处理。具体的，市售水性苯乙烯丙烯酸树脂、水性苯乙烯马来酸酐树脂和交联剂的固含量范围通常都在30wt％至40wt％，因此对应液态市售品的重量比例与实际固形物的重量比基本一致，相同工艺条件下使用固定品种有机颜料色粉和基础树脂制备的核壳结构改性色粉的树脂核壳厚度与色粉粒径的比例范围也相对固定。
进一步的方案是，步骤S2中将滤液置于80℃至100℃的温度条件下蒸干。
进一步的方案是，步骤S2和S4中使用锆珠填充量为70％至80％且锆珠粒径为0.3mm的研磨机研磨处理第一分散液或第二分散液。
在同等重量下，且符合上述分子式的基础树脂所含亲和基团的数量远多于有机颜料色粉颗粒所含的亲和基团的数量，因此将有机颜料色粉作为母粒，以该树脂进行表面改性后形成的核壳结构改性色粉颗粒表面具备更多锚固点。并且上述基础树脂相比墨水、色浆领域的其他树脂具备更好的亲水性，与之对应的改性色粉还具备再分散性。因此上述改性色粉相比普通有机颜料色粉能够吸附更多分散剂，应用于色浆后色粉颗粒具备更好的亲水性、分散性和稳定性，即使储存较长时间也不易发生团聚，可明显改善色浆的储存稳定性。
其中，符合酸值在100以上的这一条件的基础树脂参与构成的树脂核壳可提高改性色粉的分散性能。基础树脂中亲和基团在Tg(玻璃化温度)值附近的温度条件下具备较强活性，因此改性色粉在研磨制备的过程中需将基础树脂加热至Tg值附近，50℃以上的Tg明显高于室温及喷墨打印墨水的工作温度，有利于提高色浆的储存稳定性和喷射性能。
苯乙烯丙烯酸树脂和苯乙烯马来酸酐树脂透光性好，对应的树脂核壳几乎不影响色粉显色，并且单位重量的两类树脂所含亲水性基团的数量较多，对应的树脂核壳可显著改善有机颜料色粉的分散性和储存稳定性。
在上述一定比例关系的改性色粉与阴离子型分散剂可稳定吸附结合，符合上述配比的颜料色浆具备稳定的分散体系且具有良好的储存稳定性。
上述具体型号的阴离子型分散剂与基础树脂通过范德华力及离子间的引力稳定结合，同时分散剂的链段伸展在溶剂中，在改性色粉粒子表面可形成厚度＞100A的分散位阻层，可有效防止改性色粉粒子发生团聚，且不会显著改变色浆黏度影响过滤性能。
较低粘度的水性颜料色浆适合制备低粘度墨水，表面张力较高的色浆对应的墨水能够更好地适应高速打印，较小平均粒径的色浆不易发生堵头。
在水性颜料色浆的制备方法中，步骤S2在适宜的温度条件、转速条件及研磨时长下可保证树脂基础树脂与交联剂充分交联并包覆于有 机颜料色粉粒子表面形成具备核壳结构的改性色粉。步骤S4通过长时间的研磨处理可保证改性色粉充分吸附阴离子型分散剂并与其他成分形成稳定的分散体系，再经离心和过滤处理后可得到粒度均匀且平均粒径较为理想的色浆。
步骤S2中，采取较低的温度蒸干滤液可有效保护改性色粉，防止树脂核壳受热变性或发生熔化粘连。
步骤S2和步骤S4中，分别采用上述粒径规格的锆珠且填充量符合上述要求的研磨机对于第一分散液和第二分散液可起到较好的研磨效果，从而将色浆成品的平均粒径控制在理想范围内。
本发明依照以下步骤制备水性颜料色浆：
S1：按重量百分比计将30％至50％的有机颜料色粉、5％至10％的基础树脂、1％至4％的交联剂和余量水性有机溶剂在室温下以800rpm至1200rpm的转速搅拌混合30min至60min得到第一分散液，基础树脂为水性苯乙烯丙烯酸树脂或水性苯乙烯马来酸酐树脂，交联剂为多异氰酸酯交联剂。
S2：将第一分散液在基础树脂玻璃化温度±5℃的温度条件及2000rpm至2500rpm的转速条件下使用卧式研磨机研磨处理2h至3h后用0.45μm孔径滤膜过滤，卧式研磨机使用0.3mm粒径锆珠且锆珠的填充量为70％至80％，取滤液在80℃至100℃温度条件下蒸干后放入颜料粉碎机粉碎并过500目筛得到改性色粉。
S3：按重量百分比计将10％至30％的改性色粉、5％至10％的水性有机溶剂、3％至5％的阴离子型分散剂、0.5％至2％的助剂组合物以及余量水在室温下以800rpm至1200rpm的转速搅拌混合1h至2h得到第二分散液，助剂组合物包括pH调节剂、消泡剂和杀菌剂。
S4：将第二分散液在室温及1500rpm至2000rpm的转速条件下使用卧式研磨机研磨处理4h至6h，卧式研磨机使用0.3mm粒径锆珠且锆珠的填充量为70％至80％，随后在6000rpm至8000rpm的转速条件下离心10min至20min，最后经1.0μm孔径滤膜过滤得到水性颜料色浆。
实施例一至四
实施例一至四均按照上述方法制备水性颜料色浆，涉及的改性色粉及色浆的具体成分配比参见表1和表2。实施例中使用科莱恩的BG-NIP PV FAST BLUE(青)、INK jet MAGENTA E02(品红)、INK jet Yellow 4GC(黄)以及BASF的Paliotol Black L0080(黑)作为有机颜料色粉；使用日本星光PMC的HIROS X-1水性苯乙酸丙烯酸树脂和荷兰POLYSCOPE的XIRAN 1000H水性苯乙烯马来酸酐树脂作为基础树脂，两种基础树脂的酸值均在100以上，Tg均在50℃以上。
另外，多异氰酸酯交联剂使用JETIC公司的IT AD201D；阴离子型分散剂选用德国毕克的BYK 190、BYK 192和美国气体化学的ZetaSperse 3100、ZetaSperse 3700；水溶性有机溶剂使用丙二醇，pH调节剂使用三乙醇胺，消泡剂使用德国毕克的BYK-094，杀菌剂使用TROY公司的MERGAL K10N。
表1：改性色粉成分表
表2：水性颜料色浆成分表
取A至D组制备的改性色粉以及对应的有机颜料色粉各5g，分别洒入8个盛有100ml去离子水的烧杯中，用玻璃棒搅拌后静置并观察分散状态，四种有机颜料色粉颗粒在水中散开后又呈现出团聚状态，而四种改性色粉颗粒均能一直保持散开状态，说明通过上述方法进行表面改性后可使色粉颗粒表面具备一定的亲水性且不易发生团聚，从而达到了预期的改性目的。
经检测实施例一至四制备的水性颜料色浆的粘度均在2cP至10cP，表面张力均在35mN/m至70mN/m，平均粒径均在100nm至130nm。
墨水色密度测试
取实施例一至四制备的四色水性颜料色浆，以及市售主流厂商的四色水性颜料色浆成品按相同方法分别制备水性颜料墨水，水性颜料墨水的制备方法如下：
按重量百分比计取30％的颜料色浆、10％的丙烯酸树脂、1.0％的炔二醇表面活性剂、0.1％的杀菌剂和余量水，室温下以1000rpm的转速搅拌混合60min后，经过0.45μm孔径滤膜过滤。其中，丙烯酸树脂选用荷兰帝斯曼的NeoCryl BT-107-S，炔二醇表面活性剂选用美国气体化学的Surfynol 465，杀菌剂使用TROY公司的MERGAL K10N。
取上述墨水利用黑迈P-PRESS数码直喷印花机按照100％喷墨设置在白色纯棉布料上打印单一色块，随后使用X-RITE 528测色仪对打印色块进行色密度测试，测试结果见表3。表3中，对比例使用的墨水均由市售色浆制备，相同编号的实施例与对比例采用相同颜色的色浆制备墨水。从表3可以看出，采用实施例一至四的色浆制备的墨水与市售色浆产品制备的墨水在L值(表征黑白，“+”表示偏白，“-”表示偏暗)、a值(表征红绿，“+”表示偏红，“-”表示偏绿)和b值(表征黄蓝，“+”表示偏黄，“-”表示偏蓝)上均十分接近，因此在显色效果上基本一致。
表3：色密度测试结果
墨水打印流畅性测试
取“墨水色密度测试”中对应于实施例一至四的水性颜料墨水各500ml，利用EPSON 4720打印机按照单一色块，100％喷墨设置连续打印，边打印边进行观察，打印介质为纸张。
观察发现实施例一至四对应的水性颜料墨水，可连续打印500ml，打印流畅无白线，证明本发明制备的水性颜料色浆对应的水性颜料墨水的喷射性能良好，因此本发明制备的水性颜料色浆可用于制备喷墨打印墨水。
色浆储存稳定性测试
将实施例一至四制备的水性颜料色浆及“墨水色密度测试”中使用的市售色浆置于60℃恒温箱内老化四周，每种色浆在老化处理前后均测试pH值、电导率、表面张力、粘度和粒径并计算相应的变化率，变化率低于5％才可判为合格，检测结果见表4。表4中D50值代表累计粒度分布百分数达到50％时所对应的粒径，即粒径大于该值的颗粒占50％，小于它的颗粒也占50％，D90值的定义也遵循相似的逻辑。表4中计算变化率时是取老化前后各检测项下检测值之差的绝对值除以老化前对应检测项的检测值。从表4可以看出，实施例一至四对应的色浆在pH值、电导率、表面张力、粘度和粒径检测项下的储存稳定性测试全部合格，并且在绝大多数检测项下的变化率都优于市售色浆，表明本发明制备的水性颜料色浆具备较好的储存稳定性。
表4：储存稳定性测试结果
最后需要强调的是，本发明不限于上述实施方式，如各组分含量的改变等变化也应该包括在本发明权利要求的保护范围内。
工业应用性
本发明用于制备得到储存稳定性更好的水性颜料色浆，并且使该种水性颜料色浆的亲水性、分散性和稳定性更好。本发明中的水性颜料色浆中选用的色粉具有在分散性，选用的基础树经改性后形成的核壳结构改性色粉颗粒，使其表面具备更多锚固点，从而使色粉储存长时间不易发生团聚，从而改善色浆的储存稳定性。通过进一步地选用酸值在100以上且玻璃化温度在50℃以上的基础树脂、多异氰酸酯交联剂、阴离子型分散剂，并且控制水性颜料色浆各组分的用量，使得色浆的粘度、表面张力以及平均粒径控制在一定范围内，再通过制备色浆时通过控制适宜的温度、转速、研磨时长等制备条件，使制备得到的色浆具备稳定的分散体系且具有良好的储存稳定性，本发明的水性颜料色浆广泛应用于水性墨水体系的着色中，保证墨水的品质及其喷射性能。
Claims (9)
- 一种水性颜料色浆，其特征在于：包括改性色粉，所述改性色粉包括有机颜料色粉和树脂核壳，所述树脂核壳由基础树脂与交联剂共聚得到，所述基础树脂的分子式为：
其中，R1为甲基或氢，R2为烷基或烯基。 - 如权利要求1所述的水性颜料色浆，其特征在于：所述基础树脂的酸值在100以上，所述基础树脂的玻璃化温度在50℃以上。
- 如权利要求1所述的水性颜料色浆，其特征在于：所述基础树脂为水性苯乙烯丙烯酸树脂或水性苯乙烯马来酸酐树脂，所述交联剂为多异氰酸酯交联剂。
- 如权利要求1至3中任意一项所述的水性颜料色浆，其特征在于：按重量百分比计包括10％至30％的改性色粉、5％至10％的水溶性有机溶剂、3％至5％的阴离子型分散剂、0.5％至2％的助剂组合物，余量为水，所述助剂组合物包括pH调节剂、消泡剂和杀菌剂。
- 如权利要求4所述的水性颜料色浆，其特征在于：所述阴离子型分散剂选自BYK 190、BYK 192、ZetaSperse 3100、ZetaSperse 3700中的一种或两种。
- 如权利要求4所述的水性颜料色浆，其特征在于：该水性颜料色浆的粘度为2cP至10cP，表面张力为35mN/m至70mN/m，平均粒径为100nm至130nm。
- 如权利要求4至6中任意一项所述的水性颜料色浆的制备方法，其特征在于，包括下列步骤：S1：按重量百分比计将30％至50％的有机颜料色粉、5％至10％的基础树脂、1％至4％的交联剂和余量水性有机溶剂在室温下以800rpm至1200rpm的转速搅拌混合30min至60min得到第一分散液；S2：将所述第一分散液在所述基础树脂的玻璃化温度±5℃的温度条件及2000rpm至2500rpm的转速条件下研磨处理2h至3h后用0.45μm孔径滤膜过滤，取滤液蒸干后粉碎并过500目筛得到改性色粉；S3：按重量百分比计将10％至30％的改性色粉、5％至10％的水性有机溶剂、3％至5％的阴离子型分散剂、0.5％至2％的助剂组合物以及余量水在室温下以800rpm至1200rpm的转速搅拌混合1h至2h得到第二分散液；S4：将所述第二分散液在室温及1500rpm至2000rpm的转速条件下研磨处理4h至6h后在6000rpm至8000rpm的转速条件下离心10min至20min，再经1.0μm孔径滤膜过滤后取滤液。
- 如权利要求7所述的水性颜料色浆的制备方法，其特征在于：步骤S2中将所述滤液置于80℃至100℃的温度条件下蒸干。
- 如权利要求7所述的水性颜料色浆的制备方法，其特征在于：步骤S2和S4中使用锆珠填充量为70％至80％且锆珠粒径为0.3mm的研磨机研磨处理所述第一分散液或所述第二分散液。
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| CN117720838A (zh) * | 2023-12-16 | 2024-03-19 | 广州市美帮祈富文仪有限公司 | 一种高分散性的绘画用丙烯颜料色浆及其制备方法 |
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| CN112552746A (zh) * | 2020-11-30 | 2021-03-26 | 珠海天威新材料股份有限公司 | 一种水性颜料色浆及其制备方法 |
| CN114524941B (zh) * | 2022-02-25 | 2023-03-28 | 肇庆市欧陶新型材料有限公司 | 一种氮/硫杂化改性苯马树脂陶瓷分散剂及其制备方法和应用 |
| CN114736533B (zh) * | 2022-04-13 | 2023-11-17 | 苏州世名科技股份有限公司 | 表面改性有机颜料及改性方法、应用和包含其的色母粒 |
| CN116376314A (zh) * | 2023-04-13 | 2023-07-04 | 宇虹颜料股份有限公司 | 一种在水性应用中具有高着色力、高透明度的颜料制备方法 |
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