High-grinding-efficiency color paste, preparation method thereof and dispersed ink

Abstract

The invention provides high-grinding-efficiency color paste, a preparation method thereof and dispersed ink, and belongs to the technical field of dispersed ink, and the high-grinding-efficiency color paste comprises the following components in percentage by weight: 15%-30% of disperse dye toner, 15%-25% of a dispersing agent, 5%-15% of resin ammonium salt, 10%-20% of a dissolution promoting mixture, 0.5%-2% of a wetting agent and the balance of water; the dispersing agent comprises a hyperbranched polymer and a sodium naphthalene sulfonate improved polymer; the hyperbranched polymer takes a benzene ring as a center, hydrophobic groups and hydrophilic groups on a branched chain are randomly distributed, the hydrophilic groups of the branched chain comprise carboxylate and sulfonate, and the hydrophobic groups of the branched chain comprise alkane, ester and aryl. According to the invention, the hyperbranched polymer and the sodium naphthalene sulfonate improved polymer are mixed with the dispersing agent, so that the problem of abrupt change of ink viscosity can be avoided when the content of ink toner is relatively high, thereby obtaining the color paste with strong dispersion and high stability, and further obtaining the dispersed ink with good stability.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of dispersion ink, and particularly relates to a high-grinding-efficiency color paste, a preparation method thereof and dispersion ink. BACKGROUND

[0002] In the digital textile printing industry, dispersion ink is dyed in a dispersed state during printing and dyeing due to its small molecules, simple structure and non-ionizable water-soluble groups. Compared with traditional dispersion dye color paste, dispersion ink overcomes the dilemma of high energy consumption, high pollution, high emission and low efficiency of traditional dispersion dye color paste, and the fastness of the printed product is good. However, with the increasing strictness of environmental protection requirements, many color paste manufacturers have reduced the synthesis of color paste and subsequent impurity removal process to some extent in order to reduce production costs, which leads to high salt content and high impurity content in the original powder in the dispersion ink market, affecting the stability of the DLVO double electric layer, and false plasticity is easily formed during grinding, and the product quality is unstable.

[0003] In the production process of color paste, dispersion dye color paste needs to be ground to nano particles, and the grinding quality directly determines the quality of the color paste. The dispersion dye itself is not water-soluble, and the traditional grinding formula uses glycerol aqueous solution as the grinding material base solution. The dispersion dye is extremely slow to emulsify and wet, and the dispersion dye that is not completely wet has multiple crystal forms that are extremely difficult to disperse and grind, which greatly limits the grinding efficiency. At the same time, the single use of the dispersant sodium lignosulfonate or the related modified dispersant will cause a sudden change in the viscosity of the ink due to the hydrolysis of the lignin dispersant when the content of the ink color paste is high. Therefore, it is impossible to obtain a color paste with strong dispersion and high stability, and it is also impossible to obtain an ink with good stability.

[0004] Therefore, it is urgent to develop a method for grinding high-salt dispersion dyes with high grinding efficiency and a process for preparing dispersion ink to solve the above problems and improve the product quality stability of dispersion ink. SUMMARY

[0005] In view of the technical problems in the background art, the present application provides a high-grinding-efficiency color paste, a preparation method thereof and dispersion ink, which aims to solve the technical problems that the existing color paste is easy to be grinded and the dispersion ink prepared has poor stability.

[0006] In a first aspect, the present application provides a high-grinding-efficiency color paste, which comprises, by weight percentage: 15% to 30% of dispersion dye color paste, 15% to 25% of dispersant, 5% to 15% of resin ammonium salt, 10% to 20% of solubility-promoting mixture, 0.5% to 2% of wetting agent, and the balance of water. The dispersant comprises an ultrabranched polymer and a sodium naphthalenesulfonate modified polymer. The hyperbranched polymer is centered on a benzene ring, and the hydrophobic groups and the hydrophilic groups are randomly distributed on the branches, the hydrophilic groups of the branches include carboxylate and sulfonate, and the hydrophobic groups of the branches include alkyl, ester and aromatic hydrocarbon groups Preferably, the hyperbranched polymer has the structural formula: , wherein a is an integer between 10 and 50, b is an integer between 10 and 50, c is an integer between 10 and 50, d is an integer between 10 and 50, e is an integer between 10 and 50, and f is an integer between 10 and 50.

[0007] Preferably, the hyperbranched polymer has a molecular weight of 20,000-40,000, and the anionic monomer content in the hyperbranched polymer is 2-2.3 mmol / g.

[0008] Preferably, the mass ratio of the hyperbranched polymer to the sodium naphthalene sulfonate modified polymer is (2-5):1.

[0009] Preferably, the sodium naphthalene sulfonate modified polymer includes at least one of sodium alkyl naphthalene sulfonate formaldehyde polycondensate, sodium methyl naphthalene sulfonate formaldehyde polycondensate, beta-sodium naphthalene sulfonate formaldehyde condensate and sodium alkyl naphthalene sulfonate formaldehyde polycondensate.

[0010] Preferably, the solubilizing mixture includes at least three of polyhydric alcohol, amide compound, glycol ether and cyclic alkyl ester.

[0011] Preferably, the resin ammonium salt includes at least one of polyacrylamide, polyurethane ammonium salt and polyester ammonium salt; and the wetting agent includes at least one of BYK333, BYK345, S-465, FS100.

[0012] In a second aspect, the present application provides a preparation method of high-grinding-efficiency color paste, including the following steps: mixing the dispersion dye color powder, the dispersant, the resin ammonium salt, the solubilizing mixture, the wetting agent and water uniformly, and performing grinding treatment to obtain the high-grinding-efficiency color paste; wherein the grinding time is 2-4 h, the grinding temperature is 25-35 DEG C, and the grinding pressure is 10-20 MPa.

[0013] In a third aspect, the present application provides a dispersion ink, and the preparation raw material of the dispersion ink includes the high-grinding-efficiency color paste provided in the first aspect.

[0014] Preferably, the dispersion ink includes, by weight percentage, 40-60% of the high-grinding-efficiency color paste, 10-20% of the organic solvent, 1-4% of the surfactant and the balance of water.

[0015] Compared with the prior art, the present application has the following beneficial effects: (1) The present application adopts hyperbranched polymer dispersant and sodium naphthalenesulfonate to improve the polymer mixed dispersant, when the ink toner content is high, the problem of viscosity mutation of ink caused by hydrolysis of single dispersant can be avoided, so that the strong dispersion and high stability of the color paste are obtained, and then the dispersion ink with good stability is obtained.

[0016] (2) The color paste provided by the present application introduces a solubilizing mixture, including at least three of polyol, glycol ether, amide compound and cyclic alkyl ester, which can effectively promote the dissolution of disperse dye, improve the dispersion stability and redispersion performance of disperse dye. The introduction of water-based resin such as polyacrylic acid resin ammonium salt can effectively promote the stability of double electric layer and prevent the color paste from false plasticity and slurry, so as to solve the problem of unstable product quality caused by high salt content and high impurity content in the original powder; The ratio of disperse dye toner, dispersant, resin ammonium salt, solubilizing mixture, wetting agent and water can significantly improve the grinding efficiency of disperse dye, and overcome the poor emulsification and wetting effect of traditional glycerol aqueous solution base fluid on disperse dye.

[0017] (3) The color paste formula and preparation method provided by the present application have strong universality, can be applied to the grinding of various high salt disperse dyes and the preparation of dispersion ink, and improve the flexibility of dispersion ink production and the stability of product quality. DETAILED DESCRIPTION

[0018] The embodiments of the technical scheme of the present application will be described in detail below. The following examples are only used to more clearly illustrate the technical scheme of the present application, and therefore only serve as examples, but cannot limit the protection scope of the present application.

[0019] To solve the technical problem that the color paste is easy to slurry and the dispersion ink prepared has poor stability when high-efficiency grinding is carried out on the color paste with high color powder content, the present application provides a high-grinding-efficiency color paste, a preparation method thereof and a dispersion ink, wherein the problem of viscosity mutation of ink caused by hydrolysis of single dispersant is avoided through the synergistic effect of hyperbranched polymer and sodium naphthalenesulfonate improved polymer, and a variety of solubilizing mixtures and resin ammonium salt are introduced to further improve the dispersion stability and redispersion performance of disperse dye.

[0020] In a first aspect, the present application provides a high-grinding-efficiency color paste, which comprises, by weight percentage: disperse dye toner 15%~30%, dispersant 15%~25%, resin ammonium salt 5%~15%, solubilizing mixture 10%~20%, wetting agent 0.5%~2%, and the balance being water. The dispersant comprises hyperbranched polymer and sodium naphthalenesulfonate improved polymer. The hyperbranched polymer takes benzene ring as the center, and the hydrophobic groups and hydrophilic groups on the branched chain are randomly distributed, the hydrophilic groups of the branched chain include carboxylate and sulfonate, and the hydrophobic groups of the branched chain include alkane group, ester group and aromatic hydrocarbon group.

[0021] The linear structure of the conventional dispersant results in strong intermolecular interaction, which is difficult to stretch in a non-water system, thereby affecting the dispersion effect, and may cause a sudden change in viscosity of the dispersion system during long-term use or aging, affecting the stability of the system.

[0022] In the technical scheme of the embodiment of the present application, the dispersant is compounded with the hyperbranched polymer and the sodium naphthalene sulfonate improved polymer; wherein the solvated chain of the hyperbranched structure has better stretchability in a non-water system, which makes up for the shortcomings of the conventional dispersant; the hydrophobic groups and the hydrophilic groups are randomly distributed, which increases the interface applicability of the dispersant and optimizes the steric hindrance effect; the high molecular chain is more likely to form a weak micelle structure, which can quickly migrate to the surface of the particles to complete wetting, thereby shortening the dispersion time and avoiding the problem of chain entanglement caused by too large molecular weight; the hyperbranched dispersant prevents the shedding caused by too many hydrophilic chains (such as the conventional dispersant which is easy to fail due to too strong hydrogen bond), and avoids the bridging flocculation caused by too long hydrophobic chains; the hydrophilic groups are carboxyl and sulfonic acid groups, which enhance the tolerance to hard water; high-density aromatic hydrocarbons are introduced to enhance the density of π-π conjugated electron cloud and improve the Zeta potential stability of the dispersed dye. In addition, the phenolic hydroxyl groups of the sodium naphthalene sulfonate improved polymer and the protonated amine groups of the hyperbranched dispersant produce ion-π spatial synergistic effect, which further stabilizes the dispersion interface; the aliphatic long chains introduced by the hyperbranched dispersant and the polar groups of the sodium naphthalene sulfonate improved polymer synergistically improve the compatibility of the polymer matrix, solving the problem of sudden change in viscosity after aging of a single dispersant.

[0023] Preferably, the structural formula of the hyperbranched polymer is as follows: , wherein a is an integer between 10 and 50, b is an integer between 10 and 50, c is an integer between 10 and 50, d is an integer between 10 and 50, e is an integer between 10 and 50, and f is an integer between 10 and 50.

[0024] Preferably, the molecular weight of the hyperbranched polymer is 20,000-40,000, and the anionic monomer content in the hyperbranched polymer is 2-2.3 mmol / g.

[0025] In the technical scheme of the embodiment of the present application, reasonable control of the molecular weight of the hyperbranched polymer can ensure that it forms a stable adsorption with the dye molecules, thereby ensuring the grinding efficiency; reasonable control of the anionic monomer content can ensure the hydrophilicity and prevent the hydrophilic groups from causing chain relaxation, thereby causing sudden change in viscosity of the ground color paste and pseudoplasticity.

[0026] Preferably, the mass ratio of the hyperbranched polymer to the sodium naphthalene sulfonate improved polymer is (2-5):1.

[0027] In the technical scheme of the embodiment of the present application, the content of the hyperbranched polymer is further increased by adjusting the ratio of the hyperbranched polymer and the sodium naphthalene sulfonate, so as to further enhance the synergistic effect of the two. When the content of the hyperbranched polymer is too low, the sanding efficiency is reduced, and the viscosity of the ground color paste is reduced. When the content of the hyperbranched polymer is too high, the production cost is greatly increased, the grinding viscosity is too high, and the hyperbranched structure is easily embedded in the small molecule surfactant, so as to weaken the electrostatic effect. When the two are compounded, the ratio needs to be optimized to ensure that the electrostatic and steric hindrance synergistic effect takes effect.

[0028] Preferably, the mass ratio of the hyperbranched polymer and the sodium naphthalene sulfonate is 3:1.

[0029] Preferably, the sodium naphthalene sulfonate polymer includes at least one of alkyl naphthalene sulfonate formaldehyde condensate, methyl naphthalene sulfonate formaldehyde condensate, beta-naphthalene sulfonate formaldehyde condensate, and alkyl naphthalene sulfonate formaldehyde condensate.

[0030] Preferably, the solubilizing mixture includes at least three of polyhydric alcohol, amide compound, glycol ether, and cyclic alkyl ester.

[0031] Preferably, the polyhydric alcohol includes at least one of polyethylene glycol 400, ethylene glycol, 1,5-pentanediol, diglycerol, polyvinyl alcohol, diethylene glycol, 1,2-butanediol, 1,4-butanediol, glycerol, 1,2-propanediol, and 1,3-propanediol.

[0032] Preferably, the amide compound includes at least one of polyvinylpyrrolidone, N-methylpyrrolidone, alpha-pyrrolidone, and N-ethylpyrrolidone.

[0033] Preferably, the glycol ether includes at least one of diethylene glycol, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monobutyl ether, dipropylene glycol monoethyl ether, and tripropylene glycol monomethyl ether.

[0034] Preferably, the cyclic alkyl ester includes at least one of pentyl lactate, butyric acid lactone, butenolide, hexyl lactone, and heptyl lactone.

[0035] In the technical scheme of the embodiment of the present application, the dispersion dye toner is a commercially available toner of different colors, for example, the cyan pigment can be selected from any one of dispersion blue 56, dispersion blue 82, dispersion blue 60, dispersion blue 359, dispersion blue 360, dispersion blue 183, dispersion blue 354, dispersion blue 165, and dispersion blue B; the yellow pigment can be selected from any one of dispersion yellow 64, dispersion yellow 118, dispersion yellow 119, dispersion yellow 114, dispersion yellow 211, and dispersion yellow 241.

[0036] Preferably, the resin ammonium salt includes at least one of polyacrylammonium salt, polyurethane ammonium salt, and polyester ammonium salt.

[0037] Preferably, the wetting agent includes at least one of BYK333, BYK345, S-465, FS100 of BASF.

[0038] Preferably, the particle size of the disperse dye toner in the high grinding efficiency colorant is 100-200 nm.

[0039] In a second aspect, the embodiment of the present application provides a preparation method of high grinding efficiency colorant, comprising the following steps: mixing disperse dye toner, dispersant, resin ammonium salt, solubility promoting mixture, wetting agent and water uniformly, and performing grinding treatment to obtain high grinding efficiency colorant; wherein the grinding time is 2-4 h, the grinding temperature is 25-35℃, and the grinding pressure is 10-20 MPa.

[0040] In a third aspect, the embodiment of the present application provides a disperse ink, which comprises 40-60% of high grinding efficiency colorant, 10-20% of organic solvent, 1-4% of surfactant and the balance of water by weight percentage.

[0041] Preferably, the organic solvent includes at least one of ethylene glycol, glycerol, diethylene glycol, triethylene glycol and polyethylene glycol.

[0042] Some specific examples are listed below, it should be noted that the examples described below are exemplary and are only used to explain the present application, and cannot be understood as a limitation of the present application. If the specific technology or condition is not specified in the examples, the technology or condition described in the literature in the art or according to the product manual is used. If the reagent or instrument is not specified by the manufacturer, it is a conventional product that can be obtained by market purchase.

[0043] In the following examples 1-5, the preparation method of the hyperbranched polymer is as follows: (1) Cylclohexylamine (10 mmol) and glycerol (12 mmol) were dissolved in anhydrous tetrahydrofuran (THF), cooled to 0℃ in an ice bath, and acetic anhydride (12 mmol) was added dropwise to catalyze the reaction to generate cylclohexylamine-monacetylated glycerol (with two hydroxyl groups remaining), and the solvent was removed by reduced pressure distillation, and column chromatography separation (eluent: ethyl acetate / petroleum ether=7:3) purification.

[0044] (2) Acrylate modification: Acrylic acid (15 mmol) and DCC (dicyclohexyl carbodiimide) (15 mmol) were activated in THF for 30 minutes, and the above core molecule (cylclohexylamine-monacetylated glycerol) was added, and reacted at 25℃ for 12 hours to generate hyperbranched core monomer (HBP-core) containing double bonds. The formation of ester bond (1720 cm -1 ) and double bond (1635 cm -1 ) was confirmed by FT-IR.

[0045] (3) cyclohexylamine (11 mmol) and maleic anhydride (10 mmol) are dissolved in ethanol, slowly warmed to 80°C for 2 hours, and then a catalyst BF3·Et2O is added and warmed to 100°C for 2 hours. A white crystalline N-cyclohexyl maleimide is obtained by filtration.

[0046] (4) Hyperbranched copolymerization: The reaction monomers HBP-core (1.0 g), styrene (5 g), sodium styrene sulfonate (2 g), acrylic acid (3 g), ethylene (1.1 g), and N-cyclohexyl maleimide (1 g) are mixed and dissolved in an ethanol / water mixed solvent (volume ratio 1:1). A polymerization inhibitor HQ (200 ppm) is added to prevent double bond self-polymerization. An initiator azobisisobutyronitrile (AIBN, 1% of the total mass of monomers) is added. The system is deoxygenated by nitrogen for 30 minutes, and then warmed to 70°C. The AIBN solution is added dropwise in three portions with an interval of 1 hour. The reaction is carried out for 8 hours. The branching control is achieved by adjusting the branching density through the multiple reaction sites of HBP-core and the proportions of styrene, acrylic acid, sodium styrene sulfonate, ethylene, and N-cyclohexyl maleimide. The preferred molar ratio is HBP-core:styrene:acrylic acid:sodium styrene sulfonate:ethylene:N-cyclohexyl maleimide = 1:20:5:10:4:2. The reaction is terminated by adding mercaptoacetic acid, and then cooled to room temperature. The product is purified by dialysis (molecular weight cut-off 5000 Da) and freeze-dried to obtain a white solid. The pH is adjusted to 7-8 using NaOH to ensure complete ionization of the sulfonic acid group and the carboxyl group.

[0047] The final molecular weight is measured to be 32000-34000, and the anionic monomer content is 2-2.3 mmol / g. The structure of the obtained hyperbranched polymer is as follows: .

[0048] In the following examples of the present application, the naphthalene sulfonate formaldehyde polycondensate is Demol N from Japan Kao, the β-naphthalene sulfonate formaldehyde condensate dispersant is DYWELL-1000 from South Korea KG, the alkyl naphthalene sulfonate formaldehyde polycondensate is D425 from the United States Dow Chemical, and the polyacrylamide salt is SRT3069 from THYON.

[0049] I. Preparation method Example 1 A high grinding efficiency color paste, which includes, by weight percentage, dispersed dye color powder (disperse blue 60) 20%, hyperbranched polymer dispersant 13.3%, naphthalene sulfonate formaldehyde polycondensate 6.7%, polyacrylamide salt 10%, ethylene glycol 6%, diethylene glycol monomethyl ether 5%, N-methyl pyrrolidone 5%, wetting agent (BYK333) 1%, and deionized water 33%.

[0050] The preparation method of the high grinding efficiency color paste is as follows: according to the formula amount, the dispersion dye color powder, the hyperbranched polymer dispersant, the sodium naphthalene sulfonate formaldehyde condensate dispersant, the polyacrylate ammonium salt, the ethylene glycol, the diethylene glycol monomethyl ether, the N-methyl pyrrolidone, the wetting agent and the water are uniformly mixed, grinding treatment is carried out, the grinding time is 4 h, the grinding temperature is 30 DEG C, and the grinding pressure is 0.5 MPa, so that the high grinding efficiency color paste is obtained.

[0051] The particle size of the dispersion dye color powder in the high grinding efficiency color paste is 110 nm.

[0052] Example 2 A high grinding efficiency color paste, the formula of which is calculated according to the weight percentage, includes dispersion dye color powder (disperse blue 60) 20%, hyperbranched polymer dispersant 15%, sodium naphthalene sulfonate formaldehyde condensate dispersant 5%, polyacrylate ammonium salt 10%, ethylene glycol 6%, diethylene glycol monomethyl ether 5%, N-methyl pyrrolidone 5%, wetting agent (BYK333) 1%, and deionized water 33%.

[0053] The preparation method of the high grinding efficiency color paste is the same as that in example 1.

[0054] The average particle size of the dispersion dye color powder in the high grinding efficiency color paste is 118 nm.

[0055] Example 3 A high grinding efficiency color paste, the formula of which is calculated according to the weight percentage, includes dispersion dye color powder (disperse blue 60) 20%, hyperbranched polymer dispersant 16.7%, sodium naphthalene sulfonate formaldehyde condensate dispersant 3.3%, polyacrylate ammonium salt 10%, ethylene glycol 6%, diethylene glycol monomethyl ether 5%, N-methyl pyrrolidone 5%, wetting agent (BYK333) 1%, and deionized water 33%.

[0056] The preparation method of the high grinding efficiency color paste is the same as that in example 1.

[0057] The average particle size of the dispersion dye color powder in the high grinding efficiency color paste is 115 nm.

[0058] Example 4 A high grinding efficiency color paste, the formula of which is calculated according to the weight percentage, includes dispersion dye color powder (disperse yellow 118) 25%, hyperbranched polymer dispersant 15%, beta-naphthalene sulfonate formaldehyde condensate 5%, polyacrylate ammonium salt 15%, 1,5-pentanediol 5%, butenolide 5%, N-methyl pyrrolidone 5%, wetting agent (Wingtech S-465) 1%, and deionized water 24%.

[0059] The preparation method of the high grinding efficiency color paste comprises the following steps: according to the formula amount, the dispersion dye color powder, the hyperbranched polymer dispersant, the β-naphthalenesulfonic acid sodium formaldehyde condensate dispersant, the polyacrylate ammonium salt, the 1,5-pentanediol, the butenolide, the N-methyl pyrrolidone, the wetting agent and water are uniformly mixed, grinding treatment is carried out, the grinding time is 4h, the grinding temperature is 30 DEG C, and the grinding pressure is 20MPa, so that the high grinding efficiency color paste is obtained.

[0060] The average particle size of the dispersion dye color powder in the high grinding efficiency color paste is 125nm.

[0061] Example 5 A high grinding efficiency color paste, the formula comprises the following components in percentage by weight: dispersion dye color powder (disperse yellow 118) 15%, hyperbranched polymer dispersant 12%, alkyl naphthalene sulfonic acid sodium formaldehyde condensate 4%, polyacrylate ammonium salt 10%, ethylene glycol 6%, diethylene glycol monomethyl ether 5%, N-methyl pyrrolidone 5%, caprolactone 4%, wetting agent (BYK333) 1% and deionized water 38%.

[0062] The preparation method of the high grinding efficiency color paste comprises the following steps: according to the formula amount, the dispersion dye color powder, the hyperbranched polymer dispersant, the alkyl naphthalene sulfonic acid sodium formaldehyde condensate dispersant, the polyacrylate ammonium salt, the ethylene glycol, the diethylene glycol monomethyl ether, the N-methyl pyrrolidone, the caprolactone, the wetting agent and water are uniformly mixed, grinding treatment is carried out, the grinding time is 4h, the grinding temperature is 30 DEG C, and the grinding pressure is 0.5MPa, so that the high grinding efficiency color paste is obtained.

[0063] The average particle size of the dispersion dye color powder in the high grinding efficiency color paste is 124nm.

[0064] Comparative example 1 A high grinding efficiency color paste, the formula comprises the following components in percentage by weight: dispersion dye color powder (disperse blue 60) 20%, hyperbranched polymer dispersant 20%, polyacrylate ammonium salt 10%, ethylene glycol 6%, diethylene glycol monomethyl ether 5%, N-methyl pyrrolidone 5%, wetting agent (BYK333) 1% and deionized water 33%.

[0065] The preparation method of the high grinding efficiency color paste comprises the following steps: according to the formula amount, the dispersion dye color powder, the hyperbranched polymer dispersant, the polyacrylate ammonium salt, the ethylene glycol, the diethylene glycol monomethyl ether, the N-methyl pyrrolidone, the wetting agent and water are uniformly mixed, grinding treatment is carried out, the grinding time is 4h, the grinding temperature is 30 DEG C, and the grinding pressure is 0.5MPa, so that the high grinding efficiency color paste is obtained.

[0066] The high grinding efficiency color paste of the comparative example is different from the high grinding efficiency color paste of example 2 in that the dispersant only contains the hyperbranched polymer.

[0067] The average particle size of the dispersed dye toner in the high grinding efficiency color paste is 118 nm.

[0068] Comparative Example 2 A high grinding efficiency color paste, the formula of which comprises, by weight percentage, 20% of dispersed dye toner (disperse blue 60), 20% of naphthalene sulfonic acid sodium formaldehyde condensate, 10% of polyacrylate ammonium salt, 6% of ethylene glycol, 5% of diethylene glycol monomethyl ether, 5% of N-methyl pyrrolidone, 1% of wetting agent (BYK333), and 33% of deionized water.

[0069] The preparation method of the high grinding efficiency color paste comprises the following steps: according to the formula, the dispersed dye toner, the naphthalene sulfonic acid sodium formaldehyde condensate dispersant, the polyacrylate ammonium salt, the ethylene glycol, the diethylene glycol monomethyl ether, the N-methyl pyrrolidone, the wetting agent, and the water are uniformly mixed, and then grinding treatment is performed, the grinding time is 4 h, the grinding temperature is 30℃, and the grinding pressure is 20 MPa, so that the high grinding efficiency color paste is obtained.

[0070] The average particle size of the dispersed dye toner in the high grinding efficiency color paste is 120 nm.

[0071] The difference between the high grinding efficiency color paste of the present comparative example and that of Example 2 lies in that the dispersant only contains naphthalene sulfonic acid sodium formaldehyde condensate.

[0072] Comparative Example 3 The difference between the present comparative example and Example 2 lies in that the hyperbranched polymer dispersant is replaced by a commercially available dispersant BYK190.

[0073] The average particle size of the dispersed dye toner in the high grinding efficiency color paste is 122 nm.

[0074] Application Examples 1-8 The high grinding efficiency color pastes prepared in Examples 1-5 and Comparative Examples 1-3 are respectively configured to obtain corresponding dispersed inks, which correspond to Application Examples 1-8, respectively.

[0075] The dispersed ink formula comprises, by weight percentage, 50% of high grinding efficiency color paste, 10% of glycerol, 10% of ethylene glycol, 2% of surfactant (BYK345), and 28% of deionized water.

[0076] Preparation of the dispersed ink: the organic solvent and the water are put into an ink preparation tank, and after being uniformly stirred, the high grinding efficiency color paste is added and stirred for 2 h, and then filtered to obtain the dispersed ink.

[0077] II. Test method 1. Aging stability test: The prepared ink is placed in a 60℃ oven for 168h, and the particle size, pH, tension, and viscosity change rate before and after aging are detected. The particle size D50 change before and after aging is within 10% for excellent, 10%-20% for general, and more than 20% for unqualified, and the tension and viscosity change rate is within 5% for qualified.

[0078] 2. Smoothness test: The prepared ink is printed with an EPSON5113 nozzle to test a 100% color block, and the printing is 100m. The broken line condition before and after printing is detected, and the broken line condition within 3 holes is qualified.

[0079] 3. Moisture retention test After the nozzle prints the ink, it is suspended in the air for 8h, and then a test strip is printed to detect the broken line condition of the test strip, and the broken line condition within 5 holes is qualified.

[0080] III. Analysis of test results of each embodiment and comparative example 1. Aging stability test results The aging stability test results of the dispersion ink prepared by application examples 1-8 are shown in Table 1.

[0081] Table 1

[0082] As shown in Table 1, the dispersion ink prepared by the application has good aging stability, and the viscosity, tension, and particle size change little before and after aging. The application uses hyperbranched polymers and sodium naphthalenesulfonate to improve the compounding of the polymer dispersant. Sodium naphthalenesulfonate provides high charge density (-SO3 - ionization) to establish an electrostatic repulsion barrier. The hyperbranched polymer forms a thick solvation layer through the dendritic chain to enhance the steric hindrance. The combination of the two increases the energy barrier between particles by 3-5 times, significantly inhibits flocculation, and the hydrophobic core of the hyperbranched structure can shield part of the ion interference. The sulfonic acid group of sodium naphthalenesulfonate reduces the concentration of free metal ions through chelation, and together improves the salt resistance of the system, thereby meeting the requirements for high-salt dye grinding and the universality of existing dispersion colorant grinding formulations.

[0083] The data of comparative examples 1-2 show that the aging stability of single hyperbranched polymer dispersant and single sodium naphthalenesulfonate improved polymer is significantly lower than that of example 2. This is because the hyperbranched dispersant relies on the steric hindrance of the three-dimensional structure, but the surface charge density is low. In a system with high electrolyte concentration, electrostatic shielding effect easily leads to particle flocculation. The sodium naphthalenesulfonate dispersant relies on the strong ionization of the sulfonic acid group to provide electrostatic repulsion, but the molecular weight is low, and there is no effective steric hindrance layer to prevent the Brownian motion of nanoparticles from colliding and agglomerating.

[0084] 2. Smoothness test and moisture retention test results The results of the flowability test and the moisture retention test of the dispersion inks prepared in Examples 1 to 8 are shown in Table 2.

[0085] Table 2

[0086] As shown in Table 2, the dispersion inks prepared in the present application have good flowability test and moisture retention. The data of Comparative Examples 1 to 2 show that the flowability test and moisture retention of the dispersion inks prepared by using a single hyperbranched polymer dispersant and a single sodium naphthalene sulfonate to modify the polymer are obviously lower than that of Example 2, because the poor stability of the dispersion ink affects the increase of the colorant particle size, and the large particles are precipitated to form a plug during printing.

[0087] It should be noted that the present application is not limited to the above-described embodiments. The above-described embodiments are merely examples, and embodiments having substantially the same configuration and playing the same role and effect as the technical idea within the scope of the technical solution of the present application are all included in the technical scope of the present application. Furthermore, within the scope of the gist of the present application, various modifications that can be thought of by those skilled in the art, other modes constructed by combining part of the configuration elements of the embodiments are also included in the scope of the present application.

Claims

1. A high-grinding-efficiency color paste, characterized in that, By weight percentage: 15%~30% disperse dye pigment, 15%~25% dispersant, 5%~15% resin ammonium salt, 10%~20% solubilizing mixture, 0.5%~2% wetting agent, and the balance being water; The dispersant comprises a hyperbranched polymer and a sodium naphthalene sulfonate-modified polymer; The hyperbranched polymer is centered on a benzene ring, with hydrophobic and hydrophilic groups randomly distributed on the side chains. The hydrophilic groups of the side chains include carboxylates and sulfonates, while the hydrophobic groups of the side chains include alkane groups, ester groups, and aromatic groups.

2. The high-grinding-efficiency pigment paste according to claim 1, characterized in that, The structural formula of the hyperbranched polymer is: ， Where a is an integer between 10 and 50, b is an integer between 10 and 50, c is an integer between 10 and 50, d is an integer between 10 and 50, e is an integer between 10 and 50, and f is an integer between 10 and 50.

3. The high-grinding-efficiency pigment paste according to claim 2, characterized in that, The hyperbranched polymer has a molecular weight of 20,000 to 40,000; the content of anionic monomers in the hyperbranched polymer is 2 to 2.3 mmol / g.

4. The high-grinding-efficiency pigment paste according to claim 1, characterized in that, The mass ratio of the hyperbranched polymer to the sodium naphthalenesulfonate modified polymer is (2~5):

1.

5. The high-grinding-efficiency pigment paste according to claim 1, characterized in that, The sodium naphthalene sulfonate modified polymer includes at least one of alkyl naphthalene sulfonate formaldehyde condensate, methyl naphthalene sulfonate formaldehyde condensate, β-naphthalene sulfonate formaldehyde condensate, and alkyl naphthalene sulfonate formaldehyde condensate.

6. The high-grinding-efficiency pigment paste according to claim 1, characterized in that, The solubilizing mixture includes at least three of the following: polyols, amide compounds, glycol ethers, and cyclic alkyl esters.

7. The high-grinding-efficiency pigment paste according to claim 1, characterized in that, The resin ammonium salt includes at least one of polyacrylate ammonium salt, polyurethane ammonium salt, and polyester ammonium salt; the wetting agent includes at least one of BYK333, BYK345, Evonik S-465, and BASF FS100.

8. The method for preparing high-grinding-efficiency pigment paste according to any one of claims 1 to 7, characterized in that, Includes the following steps: Disperse dye powder, dispersant, resin ammonium salt, solubilizing agent, wetting agent and water are mixed evenly and then ground to obtain a high-grinding-efficiency color paste; wherein the grinding time is 2~4h, the grinding temperature is 25~35℃ and the grinding pressure is 10~20MPa.

9. A dispersible ink, characterized in that, The raw materials for preparing the disperse ink include the high-grinding-efficiency pigment as described in any one of the claims.

10. A dispersible ink according to claim 9, characterized in that, The dispersed ink comprises, by weight percentage: 40% to 60% high grinding efficiency pigment, 10% to 20% organic solvent, 1% to 4% surfactant, and the balance water.

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