CN113265177B - Color paste for color filter - Google Patents
Color paste for color filter Download PDFInfo
- Publication number
- CN113265177B CN113265177B CN202110708713.3A CN202110708713A CN113265177B CN 113265177 B CN113265177 B CN 113265177B CN 202110708713 A CN202110708713 A CN 202110708713A CN 113265177 B CN113265177 B CN 113265177B
- Authority
- CN
- China
- Prior art keywords
- parts
- weight
- reaction kettle
- color paste
- pigment powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
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
- C09D17/002—Pigment pastes, e.g. for mixing in paints in organic medium
-
- 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
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the field of coatings, in particular to color paste for a color filter, which comprises 50-65 parts by weight of an organic solvent, 15-25 parts by weight of nano pigment powder, 5-15 parts by weight of a hyperbranched pigment dispersing agent, 1-5 parts by weight of a dispersion synergist, 3-8 parts by weight of dopamine, 1-5 parts by weight of a rheology modifier, 1-5 parts by weight of a pH regulator and 0-3 parts by weight of a functional additive; wherein the particle size of the nano pigment powder is 5-30 nm. The invention overcomes the defect of poor dispersibility of color paste for a color filter in the prior art, can effectively improve the transparency of the color paste by nano pigment powder with extremely small particle size, can ensure that the toner with a small molecular structure can be dispersed into the internal gap of the color paste by the hyperbranched pigment dispersing agent, can ensure that the dispersing effect is more uniform by matching with the use of a dispersing synergist, greatly improves the storage stability of the color paste, and does not generate the phenomena of layering, caking and settlement in the storage process.
Description
Technical Field
The invention relates to the field of coatings, in particular to color paste for a color filter.
Background
The photoresist is the core of the photoetching process, is an upstream material in various application industries such as PCB (printed Circuit Board), LCD (liquid Crystal display) and semiconductors, and has wide application in the industries of circuit boards, LCD and semiconductors.
In addition to being widely used in the fields of inks, paints, plastics coloring and the like, organic pigments are also being used in the fields of color filters, inks for inkjet and the like in large quantities in recent years, and therefore, organic pigments are more strictly required to have properties such as high transparency, high contrast, good dispersibility and the like, and ordinary pigments are hardly satisfactory.
Color paste for color filter (color paste for photoresist) is one of important materials of photoresist, and the color paste for color filter is still in blank state in domestic research and development at present, so that the research and development direction of color paste for color filter is urgent to be developed in the face of huge demand gap.
Disclosure of Invention
The invention provides color paste for a color filter, aiming at overcoming the defect that the color paste in the prior art can not meet the property requirements of high transparency, high contrast, good dispersibility and the like required by the color paste for the color filter.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the color paste for the color filter comprises 50-65 parts by weight of an organic solvent, 15-25 parts by weight of nano pigment powder, 5-15 parts by weight of a hyperbranched pigment dispersing agent, 1-5 parts by weight of a dispersion synergist, 3-8 parts by weight of dopamine, 1-5 parts by weight of a rheology modifier, 1-5 parts by weight of a pH regulator and 0-3 parts by weight of a functional additive;
wherein the particle size of the nano pigment powder is 5-30 nm.
The color paste for the color filter can effectively improve the transparency of the color paste by adopting the nano pigment powder with the particle size of 5-30 nm. In addition, the pigment dispersing agent is a hyperbranched pigment dispersing agent and has a hyperbranched structure, so that toner with a small molecular structure can be dispersed into gaps in the pigment dispersing agent, the dispersing effect can be more uniform by matching with the use of a dispersion synergist, the storage stability of the color paste can be greatly improved, and the phenomena of layering, caking and sedimentation cannot occur in the storage process.
The color paste is added with a certain amount of dopamine which can be coated on the surface of the nano pigment powder, so that the surface of the pigment powder is modified, the mixing difficulty of the nano pigment powder is reduced, and the agglomeration of the nano pigment powder is prevented.
In addition, because the dispersant in the invention has a hyperbranched structure, the viscosity of the dispersant is lower compared with that of linear and crosslinked polymers, and the dispersant has good defoaming and foam inhibition effects during use, so that a large amount of bubbles generated during photoresist preparation can be prevented.
Preferably, the nano pigment powder is subjected to superfine surface modification treatment, and the steps are as follows: adding the nano pigment powder, dopamine and alkalescent aqueous solution into a high-pressure reaction kettle, and then introducing supercritical CO into the high-pressure reaction kettle2And after mixing and dissolving for a certain time, spraying the mixture in an atmospheric environment through a constant-temperature nozzle to obtain the superfine surface modified nano pigment powder.
The nano pigment powder is subjected to ultrafine surface modification treatment, the basic principle of the nano pigment powder is based on a supercritical solution rapid expansion technology, the nano pigment powder, dopamine and a weak alkaline aqueous solution can be dissolved in supercritical carbon dioxide to form a uniform solution, when the solution is sprayed out through a nozzle, strong disturbance and huge supersaturation can be generated, so that the nano pigment powder coated with dopamine is formed, and polydopamine can be formed on the surface of the nano pigment powder when the dopamine is contacted with air in an alkaline state, so that the compatibility between the nano pigment powder and a branched pigment dispersing agent is more excellent, and the dispersion of the pigment powder is facilitated.
Preferably, the pressure in the high-pressure reaction kettle is 15-30 MPa, the temperature in the reaction kettle is 65-85 ℃, the mixture is dissolved for 2-5 hours, the diameter of the constant-temperature nozzle is less than 0.5mm, the length of the constant-temperature nozzle is less than 10mm, and the temperature of the constant-temperature nozzle is 65-75 ℃.
Preferably, the pH value of the weakly alkaline water is 8.0-9.5, and the mass of the weakly alkaline water is the same as that of the nano pigment powder.
Preferably, the preparation method of the hyperbranched pigment dispersant is as follows:
(S.1) according to a molar ratio of 1: (3-3.6) adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing an organic solvent, uniformly mixing, adding a platinum catalyst in a catalyst amount, heating to 75-90 ℃, reacting for 1-5 h, and evaporating to remove the solvent to obtain an organic silicon core A, wherein the reaction formula is shown as the following formula (1):
formula (1).
(S.2) preparing a mixture according to a molar ratio of 1: (9-13) adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing an organic solvent, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting for 5-8 hours at 40-60 ℃ to obtain an organosilicon core B with a terminal group of a silicon-hydrogen structure, wherein the reaction formula is shown as the following formula (2):
formula (2).
(S.3) according to a molar ratio of 1: (9-13) adding the organosilicon core B and 2-butene-1, 4-diol into a reaction kettle containing an organic solvent, uniformly mixing, adding a platinum catalyst with a catalytic amount, reacting at 75-90 ℃ for 3-5 h, and carrying out hydrosilylation reaction again to obtain organosilicon polyol, wherein the reaction formula is shown as the following formula (3):
formula (3).
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing an organic solvent, dropwise adding chlorosulfonic acid with the molar weight 5-9 times that of the organic silicon polyol into the reaction kettle at the temperature of-10-0 ℃, heating to 65-75 ℃, stirring for 3-6 h, removing low-boiling-point substances through reduced pressure distillation, adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersant, wherein the reaction formula is shown as the following formula (4):
formula (4).
The dispersing agent used in the invention adopts a multi-step construction mode, and the organosilicon core, the alkane inner layer and the sulfonate outer layer are sequentially formed from inside to outside, so that the dispersing agent has the advantage of regular and controllable structure, the performance of the dispersing agent can be always kept consistent, and the stability of color pastes among batches is improved.
The inner core of the organic silicon structure can enable the organic silicon structure to have extremely low surface tension, so that the generation condition of foam can be damaged, and meanwhile, the organic silicon structure has good high and low temperature resistance, so that the color paste has good storage at normal temperature and good heat storage and freeze-thaw stability. The end group of the sulfonate structure can attract groups in the nano pigment powder mutually, so that the affinity with the pigment powder can be improved, the pigment powder is easier to disperse, and the agglomeration and sedimentation are prevented.
Preferably, the chemical formula of the dispersion synergist is shown in the following formula (5):
formula (5).
Preferably, the rheology modifier is one of hydrogenated castor oil, fumed silica, hydroxyethyl cellulose, HASE thickener.
Preferably, the pH regulator is one of polyethyleneimine, triethanolamine, borax, sodium carbonate, sodium bicarbonate, and urea.
Preferably, the nanopigment powder is one or more organic or inorganic powder colorants.
Preferably, the nano pigment powder comprises one or more of monoazo, disazo, condensed azo, phthalocyanine blue, phthalocyanine green and condensed ring ketone pigments.
Wherein: the green pigment includes phthalocyanine pigment, azo pigment or heterocyclic pigment; the yellow pigment includes azo type pigment, azo condensed type pigment and heterocyclic type pigment; the red pigment is selected from PR224, PR254, PR264, PR122, PR123, PR177, PR179, PR190, etc.; the blue pigment is selected from PB1, PB2, PB15, PB15:3, PB15:4, PB15:6, PB16, PB22, PB60, etc.
Preferably, the functional additive is one or more of bactericide, defoamer, antioxidant, leveling agent, lubricant, light stabilizer and antistatic agent.
Therefore, the color paste for the color filter has the following beneficial effects:
(1) the nano pigment has extremely small particle size, and can effectively improve the transparency of the color paste;
(2) the hyperbranched pigment dispersant can enable toner with a small molecular structure to be dispersed into the internal gaps, and the use of the hyperbranched pigment dispersant in combination with a dispersion synergist can enable the dispersion effect to be more uniform;
(3) the storage stability of the color paste is greatly improved, and the phenomena of layering, caking and settlement can not occur in the storage process.
Detailed Description
The invention is further described with reference to specific examples. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Wherein the chemical formula of the dispersion synergist in the examples is shown as the following formula (5):
formula (5).
The preparation method of the dispersion synergist comprises the following steps:
the preparation method of the cycloborosiloxane core can be prepared by referring to the method disclosed in application No. CN201510873071.7, and the preparation method comprises the following steps:
(1) preparation of the cycloborosiloxane core: the three-neck reaction bottle is provided with an electromagnetic stirring device, a constant-pressure dropping funnel and a three-way valve, 0.03mol of phenylboronic acid is dissolved in 50ml of tetrahydrofuran under the protection of nitrogen at 20 ℃, the mixture is placed into the constant-pressure dropping funnel, 0.15mol of methyl hydrogen dichlorosilane is placed into the three-neck reaction bottle, the phenylboronic acid is dropwise added within 30 minutes and then continues to react for 5 hours, then under the protection of nitrogen, 0.3mol of zinc oxide and 500ml of ethyl acetate are added into the reaction bottle and stirred into suspension, the solution after the previous reaction is transferred to the constant-pressure dropping funnel, the solution is dropwise added into the suspension within 30 minutes and continues to react for 12 hours after the addition is completed; filtering to remove insoluble zinc salt, washing the filtrate with water for 100ml × 2 times, and then washing with distilled water for 100ml × 2 times; drying with anhydrous sodium sulfate, filtering, distilling off ethyl acetate and tetrahydrofuran to obtain mixed cycloborosiloxane, and distilling to obtain (PhBO) (MeHSiO)3；
(2) The three-neck reaction bottle is provided with an electromagnetic stirring device, a constant pressure dropping funnel and a three-way valve, and 0.1 mol of (PhBO) (MeHSiO) is taken under the protection of nitrogen at 45 DEG C3And 10 mg of tripentafluorophenylboronane are dissolved in 50ml of toluene, the mixture is placed into a three-neck reaction bottle, then a mixed solution of 0.3mol of 1- (2-hydroxyethyl) imidazole and 20ml of toluene is added into a constant-pressure dropping funnel, the reaction is continued for 1h after the dropping is finished, and the compound shown in the formula (5) is obtained after the solvent is evaporated.
Example 1
The color paste for the color filter comprises, by weight, 50-65 parts of an organic solvent (propylene glycol methyl ether acetate), 15 parts of nano pigment powder (disazo dye-direct scarlet 4B), 5 parts of a hyperbranched pigment dispersing agent, 5 parts of a dispersion synergist, 3 parts of dopamine, 1-5 parts of a rheological modifier (hydrogenated castor oil) and 1-5 parts of a pH regulator (polyethyleneimine).
The particle size of the nano pigment powder is between 5 and 30nm, and the nano pigment powder is subjected to superfine surface modification treatment, and the method comprises the following specific steps: weighing the nano pigment powder, dopamine, alkalescent aqueous solution with the mass pH value of 8.0 and the like according to the formula, adding the nano pigment powder, the dopamine and the alkalescent aqueous solution into a high-pressure reaction kettle, and introducing supercritical CO into the high-pressure reaction kettle2And keeping the pressure in the high-pressure reaction kettle at 15Mpa and the temperature at 65 ℃, mixing and dissolving for 2h, and spraying the mixture in an atmospheric environment through a constant-temperature nozzle with the diameter of 0.3mm and the length of 5mm, wherein the temperature of the constant-temperature nozzle is 65 ℃, so as to obtain the ultrafine surface modified nano pigment powder.
The preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: 3, adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing toluene, uniformly mixing, adding a platinum catalyst in a catalyst amount, heating to 75 ℃, reacting for 1h, and evaporating a solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: 9, adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing tetrahydrofuran, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 40 ℃ for 5 hours to obtain an organosilicon core B with an end group of a silicon-hydrogen structure;
(S.3) according to a molar ratio of 1: 9, adding the organosilicon core B and 2-butylene-1, 4-diol into a reaction kettle containing toluene, uniformly mixing, adding a platinum catalyst with a catalyst amount, reacting for 3 hours at 75 ℃, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing dichloromethane, dropwise adding chlorosulfonic acid with the molar weight 5 times that of the organic silicon polyol into the reaction kettle at the temperature of-10 ℃, continuously stirring the mixture for 3 hours after the dropwise adding is finished, removing low-boiling-point substances by reduced pressure distillation, then adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersing agent.
Example 2
The color paste for the color filter comprises 65 parts by weight of an organic solvent (dipropylene glycol methyl ether), 25 parts by weight of nano pigment powder (condensed azo pigment-pigment red 214), 15 parts by weight of a hyperbranched pigment dispersing agent, 1 part by weight of a dispersion synergist, 8 parts by weight of dopamine, 5 parts by weight of a rheology modifier (hydroxyethyl cellulose), 1-5 parts by weight of a pH regulator (triethanolamine) and 3 parts by weight of a bactericide.
The particle size of the nano pigment powder is 5-30 nm, and the nano pigment powder is subjected to superfine surface modification treatment, and the method comprises the following specific steps: weighing the nano pigment powder, dopamine, alkalescent aqueous solution with the mass pH value of 9.5 and the like according to the formula, adding the nano pigment powder, the dopamine and the alkalescent aqueous solution into a high-pressure reaction kettle, and introducing supercritical CO into the high-pressure reaction kettle2And keeping the pressure in the high-pressure reaction kettle at 30Mpa and the temperature at 85 ℃, mixing and dissolving for 5 hours, and spraying the mixture in an atmospheric environment through a constant-temperature nozzle with the diameter of 0.4mm and the length of 8mm, wherein the temperature of the constant-temperature nozzle is 75 ℃, so as to obtain the ultrafine surface modified nano pigment powder.
The preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: 3.6 adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing toluene, uniformly mixing, adding a platinum catalyst with a catalyst amount, heating to 90 ℃, reacting for 5 hours, and evaporating to remove a solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: 13 adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing tetrahydrofuran, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 60 ℃ for 8 hours to obtain an organosilicon core B with an end group of a silicon-hydrogen structure;
(S.3) according to a molar ratio of 1: 13 adding the organosilicon core B and 2-butylene-1, 4-diol into a reaction kettle containing toluene, uniformly mixing, adding a catalyst amount of platinum catalyst, reacting for 5 hours at 90 ℃, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing dichloromethane, dropwise adding chlorosulfonic acid with the molar weight 9 times that of the organic silicon polyol into the reaction kettle at 0 ℃, heating to 75 ℃, stirring for 6 hours, carrying out reduced pressure distillation to remove low-boiling-point substances, then adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersant.
Example 3
The color paste for the color filter comprises, by weight, 55 parts of an organic solvent (propylene glycol methyl ether acetate), 20 parts of nano pigment powder (PB 1), 10 parts of a hyperbranched pigment dispersing agent, 3 parts of a dispersion synergist, 5 parts of dopamine, 3 parts of a rheology modifier (HASE thickener), 3 parts of a pH regulator (urea) and 2 parts of an antioxidant.
The particle size of the nano pigment powder is 5-30 nm, and the nano pigment powder is subjected to superfine surface modification treatment, and the method comprises the following specific steps: weighing the nano pigment powder, dopamine, alkalescent aqueous solution with the mass pH value of 8.5 and the like according to the formula, adding the nano pigment powder, the dopamine and the alkalescent aqueous solution into a high-pressure reaction kettle, and introducing supercritical CO into the high-pressure reaction kettle2And keeping the pressure in the high-pressure reaction kettle at 25Mpa and the temperature at 75 ℃, mixing and dissolving for 4 hours, and spraying the mixture in an atmospheric environment through a constant-temperature nozzle with the diameter of 0.4mm and the length of 8mm, wherein the temperature of the constant-temperature nozzle is 70 ℃, so as to obtain the ultrafine surface modified nano pigment powder.
The preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: 3.5 adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing an organic solvent, uniformly mixing, adding a platinum catalyst with a catalyst amount, heating to 85 ℃, reacting for 3h, and evaporating the solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: 10, adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing an organic solvent, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 50 ℃ for 7 hours to obtain an organosilicon core B with an end group of a silicon-hydrogen structure;
(S.3) according to a molar ratio of 1: 10, adding the organosilicon core B and 2-butylene-1, 4-diol into a reaction kettle containing an organic solvent, uniformly mixing, adding a platinum catalyst with a catalyst amount, reacting for 4 hours at 85 ℃, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing an organic solvent, dropwise adding chlorosulfonic acid with the molar weight 6 times that of the organic silicon polyol into the reaction kettle at the temperature of-5 ℃, heating to 70 ℃, stirring for 5 hours, carrying out reduced pressure distillation to remove low-boiling-point substances, then adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersing agent.
Example 4
The color paste for the color filter comprises, by weight, 50-65 parts of an organic solvent (propylene glycol methyl ether acetate), 18 parts of nano pigment powder (phthalocyanine green), 8 parts of a hyperbranched pigment dispersing agent, 2 parts of a dispersion synergist, 5 parts of dopamine, 1-5 parts of a rheology modifier (hydroxyethyl cellulose), 2 parts of a pH regulator (borax) and 1 part of a light stabilizer.
The particle size of the nano pigment powder is 5-30 nm, and the nano pigment powder is subjected to superfine surface modification treatment, and the method comprises the following specific steps: weighing the nano pigment powder, dopamine, alkalescent aqueous solution with the mass pH value of 8.8 and the like according to the formula, adding the nano pigment powder, the dopamine and the alkalescent aqueous solution into a high-pressure reaction kettle, and introducing supercritical CO into the high-pressure reaction kettle2Keeping the pressure in the high-pressure reaction kettle at 18Mpa and the temperature at 70 ℃, mixing and dissolving for 2.5h, then passing through a reactor with the diameter of 0.4mm,spraying out the nano pigment powder with the length of 8mm in an atmospheric environment by using a constant-temperature nozzle at the temperature of 70 ℃ to obtain the superfine surface modified nano pigment powder.
The preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: (3-3.6) adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing toluene, uniformly mixing, adding a catalyst amount of platinum catalyst, heating to 78 ℃, reacting for 1.5h, and evaporating to remove the solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: 10.5 adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing tetrahydrofuran, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 45 ℃ for 6 hours to obtain an organosilicon core B with an end group of a silicon-hydrogen structure;
(S.3) according to a molar ratio of 1: 11, adding the organosilicon core B and 2-butylene-1, 4-diol into a reaction kettle containing toluene, uniformly mixing, adding a catalyst amount of platinum catalyst, reacting at 78 ℃ for 3.5 h, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing dichloromethane, dropwise adding chlorosulfonic acid with the molar weight 5.5 times of that of the organic silicon polyol into the reaction kettle at the temperature of-2 ℃, heating to 70 ℃, stirring for 4 hours, carrying out reduced pressure distillation to remove low-boiling-point substances, then adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersing agent.
Example 5
The color paste for the color filter comprises, by weight, 60 parts of an organic solvent (propylene glycol methyl ether acetate), 24 parts of nano pigment powder (PB 15: 4), 12 parts of a hyperbranched pigment dispersing agent, 4 parts of a dispersion synergist, 5 parts of dopamine, 4 parts of a rheology modifier (hydroxyethyl cellulose), 4 parts of a pH regulator (polyethyleneimine) and 2 parts of a functional additive (antistatic agent).
The particle size of the nano pigment powder is 5-30 nm, and the nano pigment powder is subjected to superfine surface modification treatment, and the method comprises the following specific steps: weighing nanometer pigment powder and pigment powder according to the above formulaAdding the three of barbamine and alkalescent aqueous solution with the mass pH value of 9.0 and the nano pigment powder into a high-pressure reaction kettle, and then introducing supercritical CO into the high-pressure reaction kettle2And keeping the pressure in the high-pressure reaction kettle at 25Mpa and the temperature at 80 ℃, mixing and dissolving for 4 hours, and spraying the mixture in an atmospheric environment through a constant-temperature nozzle with the diameter of 0.4mm and the length of 8mm, wherein the temperature of the constant-temperature nozzle is 70 ℃, so as to obtain the ultrafine surface modified nano pigment powder.
The preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: 3.5 adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing toluene, uniformly mixing, adding a catalytic amount of platinum catalyst, heating to 88 ℃, reacting for 4h, and evaporating the solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: 12, adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing tetrahydrofuran, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 55 ℃ for 7 hours to obtain an organosilicon core B with an end group of a silicon-hydrogen structure;
(S.3) according to a molar ratio of 1: 12, adding the organosilicon core B and 2-butylene-1, 4-diol into a reaction kettle containing toluene, uniformly mixing, adding a platinum catalyst with a catalyst amount, reacting for 4 hours at 80 ℃, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing dichloromethane, dropwise adding chlorosulfonic acid with the molar weight 8 times that of the organic silicon polyol into the reaction kettle at the temperature of-5 ℃, heating to 70 ℃, stirring for 5 hours, carrying out reduced pressure distillation to remove low-boiling-point substances, then adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain the hyperbranched pigment dispersing agent.
The color paste prepared by the invention is tested for storage stability, and the testing method is tested according to the GB/T9756-2009 Standard of synthetic resin emulsion interior wall paint.
The test results are shown in table 1 below:
TABLE 1
From the data in the above table, it can be seen that the color paste for color filters of the present invention has good storage stability, can be stably stored at normal temperature and at high and low temperatures, and has no obvious change in properties after storage, so that the performance of each batch of color paste can be always consistent, and the stability of each batch of color paste can be guaranteed.
Claims (9)
1. The color paste for the color filter is characterized by comprising 50-65 parts by weight of an organic solvent, 15-25 parts by weight of nano pigment powder, 5-15 parts by weight of a hyperbranched pigment dispersing agent, 1-5 parts by weight of a dispersion synergist, 3-8 parts by weight of dopamine, 1-5 parts by weight of a rheology modifier, 1-5 parts by weight of a pH regulator and 0-3 parts by weight of a functional additive;
wherein the particle size of the nano pigment powder is 5-30 nm;
the preparation method of the hyperbranched pigment dispersant comprises the following steps:
(S.1) according to a molar ratio of 1: (3-3.6) adding methyl hydrogen cyclotrisiloxane and vinyl trimethoxy silane into a reaction kettle containing an organic solvent, uniformly mixing, adding a catalytic amount of platinum catalyst, heating to 75-90 ℃, reacting for 1-5 h, and evaporating the solvent to obtain an organic silicon core A;
(S.2) preparing a mixture according to a molar ratio of 1: (9-13) adding the organosilicon core A and dimethylchlorosilane into a reaction kettle containing an organic solvent, uniformly mixing, adding a catalyst amount of ferric chloride, and reacting at 40-60 ℃ for 5-8 h to obtain an organosilicon core B with a silicon-hydrogen structure as an end group;
(S.3) according to a molar ratio of 1: (9-13) adding the organosilicon core B and 2-butene-1, 4-diol into a reaction kettle containing an organic solvent, uniformly mixing, adding a catalytic amount of platinum catalyst, reacting at 75-90 ℃ for 3-5 h, and carrying out hydrosilylation reaction again to obtain organosilicon polyol;
(S.4) adding the obtained organic silicon polyol into a reaction kettle containing an organic solvent, dropwise adding chlorosulfonic acid with the molar weight 5-9 times that of the organic silicon polyol into the organic silicon polyol at the temperature of-10-0 ℃, stirring for 3-6 h, then carrying out reduced pressure distillation to remove low-boiling-point substances, adding alkali liquor into the reaction kettle for neutralization, and evaporating water to obtain a hyperbranched pigment dispersing agent;
the chemical formula of the dispersion synergist is shown as the following formula (5):
formula (5).
2. The color paste for color filter according to claim 1, wherein the nano pigment powder is subjected to ultra-fine surface modification treatment, and the steps are as follows: adding the nano pigment powder, dopamine and alkalescent aqueous solution into a high-pressure reaction kettle, and then introducing supercritical CO into the high-pressure reaction kettle2And after mixing and dissolving for a certain time, spraying the mixture in an atmospheric environment through a constant-temperature nozzle to obtain the superfine surface modified nano pigment powder.
3. The color paste for the color filter according to claim 2, wherein the pressure in the high-pressure reaction kettle is 15-30 MPa, the temperature in the reaction kettle is 65-85 ℃, the color paste is mixed and dissolved for 2-5 h, the diameter of the constant-temperature nozzle is less than 0.5mm, the length of the constant-temperature nozzle is less than 10mm, and the temperature of the constant-temperature nozzle is 65-75 ℃.
4. The color paste for a color filter according to claim 2 or 3, wherein the pH value of the weakly alkaline water is 8.0-9.5, and the mass of the weakly alkaline water is the same as that of the nano pigment powder.
5. The color paste according to claim 1, wherein the rheology modifier is one of hydrogenated castor oil, fumed silica, hydroxyethyl cellulose, and HASE thickener.
6. The color paste for color filter according to claim 1, wherein the pH regulator is one of polyethyleneimine, triethanolamine, borax, sodium carbonate, sodium bicarbonate, and urea.
7. The color paste for color filter according to claim 1, wherein the nano pigment powder is one or more organic or inorganic powder colorants.
8. The color paste for color filter according to claim 7, wherein the nano pigment powder comprises one or more of monoazo, disazo, condensed azo, phthalocyanine blue, phthalocyanine green and condensed ring ketone pigments.
9. The color paste for color filter according to claim 1, wherein the functional additive is a combination of one or more of a bactericide, a defoamer, an antioxidant, a leveling agent, a lubricant, a light stabilizer and an antistatic agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110708713.3A CN113265177B (en) | 2021-06-25 | 2021-06-25 | Color paste for color filter |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110708713.3A CN113265177B (en) | 2021-06-25 | 2021-06-25 | Color paste for color filter |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113265177A CN113265177A (en) | 2021-08-17 |
| CN113265177B true CN113265177B (en) | 2022-04-26 |
Family
ID=77235932
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110708713.3A Active CN113265177B (en) | 2021-06-25 | 2021-06-25 | Color paste for color filter |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113265177B (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005307196A (en) * | 2004-03-25 | 2005-11-04 | Rikogaku Shinkokai | Siloxane derivative and production method thereof |
| CN101037545A (en) * | 2006-03-14 | 2007-09-19 | 克拉里安特国际有限公司 | Pigment preparations based on PY 155 |
| CN101331193A (en) * | 2005-11-28 | 2008-12-24 | 爱克发印艺公司 | Non-aqueous pigment dispersions containing specific dispersion synergists |
| CN102295771A (en) * | 2011-05-13 | 2011-12-28 | 华东理工大学 | Hyperbranched polymer as well as modified substance thereof and application of modified substance |
| CN107384029A (en) * | 2017-07-11 | 2017-11-24 | 河北晨阳工贸集团有限公司 | A kind of water nano mill base and preparation method thereof |
| CN111303659A (en) * | 2020-04-14 | 2020-06-19 | 联仕(昆山)化学材料有限公司 | Preparation of superfine red pigment dispersion particles for color filter |
| WO2021116333A1 (en) * | 2019-12-11 | 2021-06-17 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Q-t-siloxane-based polymeric materials with high siloxane ring content and method for preparing same |
-
2021
- 2021-06-25 CN CN202110708713.3A patent/CN113265177B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005307196A (en) * | 2004-03-25 | 2005-11-04 | Rikogaku Shinkokai | Siloxane derivative and production method thereof |
| CN101331193A (en) * | 2005-11-28 | 2008-12-24 | 爱克发印艺公司 | Non-aqueous pigment dispersions containing specific dispersion synergists |
| CN101037545A (en) * | 2006-03-14 | 2007-09-19 | 克拉里安特国际有限公司 | Pigment preparations based on PY 155 |
| CN102295771A (en) * | 2011-05-13 | 2011-12-28 | 华东理工大学 | Hyperbranched polymer as well as modified substance thereof and application of modified substance |
| CN107384029A (en) * | 2017-07-11 | 2017-11-24 | 河北晨阳工贸集团有限公司 | A kind of water nano mill base and preparation method thereof |
| WO2021116333A1 (en) * | 2019-12-11 | 2021-06-17 | Empa Eidgenössische Materialprüfungs- Und Forschungsanstalt | Q-t-siloxane-based polymeric materials with high siloxane ring content and method for preparing same |
| CN111303659A (en) * | 2020-04-14 | 2020-06-19 | 联仕(昆山)化学材料有限公司 | Preparation of superfine red pigment dispersion particles for color filter |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113265177A (en) | 2021-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CA2717707C (en) | Azo pigment composition, production process of azo pigment composition, dispersion containing azo pigment composition, coloring composition and ink for inkjet recording | |
| CN101659813B (en) | Pigment dispersion, pigment photoresistor and preparation thereof | |
| CN103357346B (en) | Pigment dispersing agent, pigment dispersion liquid, colorized photoresist, and preparation and application thereof | |
| CN108034305B (en) | Ferric oxide pigment color paste and preparation method thereof | |
| CN101987925B (en) | Fine pigment composition and manufacturing method thereof | |
| CZ184497A3 (en) | Anhydrous inks and coatings containing carbonaceous products | |
| JP2006257419A (en) | Suspension | |
| CN103857752A (en) | Azo pigment, method for producing azo pigment, dispersion containing azo pigment, tinting composition and inkjet recording ink | |
| EP2569375A2 (en) | Modified pigments | |
| CN110144141A (en) | A kind of ceramic ink jet printing ink dispersing agent and its preparation method and application | |
| US20130295501A1 (en) | Surface modification of pigments and compositions comprising the same | |
| CN113265177B (en) | Color paste for color filter | |
| CN113388298B (en) | Ultrahigh alcohol-water-resistance single-component plastic coating and preparation process thereof | |
| CN102165019A (en) | Azo pigment, method for producing the azo pigment and dispersion and coloring composition containing the azo pigment | |
| CN104610783B (en) | A kind of transparent aluminium hydroxide liquid dispersion and preparation method and application | |
| EP0957136B1 (en) | Additive for a pigment containing disazo compounds, and pigment compositions containing it | |
| CN105348919A (en) | Thermal transfer printing inkjet ink composition and preparation method thereof | |
| CN101679767A (en) | Based on the C.I. pigment Blue 15: 6 pigment preparation | |
| CN113502089B (en) | Color paste for ink of water-based pen | |
| JP4802510B2 (en) | Disazo pigment composition and method for producing the same | |
| JP4759966B2 (en) | Method for producing monoazo lake pigment composition | |
| CN101565555A (en) | Rare earth complex red pigment with excellent pigment performance and application thereof | |
| JP4602029B2 (en) | Color coating solution for color filters | |
| CN105925152A (en) | Production process of metal printing plate roll coated with nano ceramic paint in advance | |
| CN101962497B (en) | Modified phthalocyanine pigment derivate dispersant, preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |