CN111138608B - Preparation method of aqueous pigment dispersion, aqueous pigment dispersion and application - Google Patents
Preparation method of aqueous pigment dispersion, aqueous pigment dispersion and application Download PDFInfo
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- CN111138608B CN111138608B CN202010056752.5A CN202010056752A CN111138608B CN 111138608 B CN111138608 B CN 111138608B CN 202010056752 A CN202010056752 A CN 202010056752A CN 111138608 B CN111138608 B CN 111138608B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
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- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- 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
- C09D17/001—Pigment pastes, e.g. for mixing in paints in aqueous medium
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- 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
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/007—Metal oxide
- C09D17/008—Titanium dioxide
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Abstract
The invention belongs to the technical field of water-based ink, and relates to a water-based pigment, in particular to a preparation method of a water-based pigment dispersion, the water-based pigment dispersion and application. The raw materials comprise, by weight, 20-50 parts of pigment, 2-10 parts of anionic polymerizable emulsifier, 3-25 parts of maleic acid monoalkyl ester polyether, 2-10 parts of hydrophobic monofunctional polymerizable monomer, 1-5 parts of hydrophobic polyfunctional polymerizable monomer, 0.05-0.5 part of oil-soluble azo free radical initiator, a proper amount of pH regulator and 50-100 parts of deionized water, and the raw materials are subjected to radical polymerization after being fully emulsified to form a layer of crosslinked dispersant coating layer on the surface of the pigment; compared with the existing method of preparing the dispersant and then preparing the aqueous pigment dispersion, the method has the characteristics of reducing production procedures, improving production efficiency and reducing cost, and the dispersant is coated on the surface of the pigment in a crosslinking manner, so that the stability is good and the application effect in the aqueous ink is good.
Description
Technical Field
The invention belongs to the technical field of water-based ink, and relates to a water-based pigment, in particular to a preparation method of a water-based pigment dispersion, the water-based pigment dispersion and application.
Background
The aqueous ink is an ink using water as a solvent or a dispersant, and contains no or a small amount of an organic solvent, and thus meets the current environmental requirements, and has been rapidly developed in recent years. However, there are still some technical limitations to the use of aqueous inks in a wider field, where stable dispersion of the pigment is a technical limitation. In the prior art, the most common pigment dispersion method is to use a dispersant to disperse the pigment in water in advance to prepare an aqueous pigment slurry or to disperse the pigment directly in the preparation of an aqueous ink. However, the technique using a dispersant still has a problem that, with the storage of an aqueous pigment slurry or an aqueous ink, a part or even a large amount of pigment aggregates due to the insufficient dispersing effect of the dispersant or the movement of pigment particles, resulting in the change and deterioration of the properties of the aqueous ink.
The industry now proposes a new aqueous pigment dispersion method, which employs a crosslinked polymer to coat the pigment after the pigment is fully dispersed, so as to form a core-shell structure with a core of the pigment and a shell of the crosslinked polymer. The pigment is coated by the cross-linked polymer, so that the aggregation caused by the contact of pigment particles can be avoided, and the cross-linked polymer is stably coated on the surface of the pigment, so that the pigment after aqueous dispersion has better stability. The method of crosslinking a carboxyl group-containing polymer with a polyfunctional epoxy compound (CN 109563367A, CN108431074A, CN 110099971A) is proposed by Kao corporation of Japan. CN108699370A proposes a process for crosslinking an alkali-soluble resin having an acid value of 40 to 300KOHmg/g and 50 to 90% of the acid groups neutralized with a basic compound with a 2-functional epoxy crosslinking agent. CN110241471A proposes that after unsaturated carbon-carbon double bond-containing polyether modified polysiloxane is used as a polymerizable dispersant to disperse a pigment, styrene, maleic anhydride and an initiator are added to carry out polymerization to coat the pigment with a polymer, and then alkanolamide is used to carry out graft modification on the pigment coated with the polymer. However, the polymer of this method is not a crosslinked structure.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an aqueous pigment dispersion. The preparation of the dispersing agent and the dispersing process of the dispersing agent to the pigment are carried out in one reaction kettle by adopting a one-pot method, and compared with the prior art that the dispersing agent is firstly prepared to disperse the pigment, the method has the characteristics of reducing the working procedures, improving the production efficiency and reducing the cost. Meanwhile, the dispersant of the invention forms a cross-linked structure to coat on the surface of the pigment, and has the characteristics of good coating effect, good dispersion stability and good high-temperature storage property.
The dispersant in the prior art is aggregated and coated on the surface of the pigment in a single molecule form, and with the increase of the storage temperature of the water-based ink or the water-based pigment dispersion, the thermal motion of the dispersant molecules is intensified, the coating effect of the dispersant on the pigment particles is weakened, so that the aggregation opportunity of the pigment particles in the collision process is greatly improved, the pigment particles are aggregated in a large amount, the water-based ink is slightly floated and bloomed, the color difference is large, and the water-based ink or the water-based pigment dispersion is seriously layered and precipitated.
The preparation method of the invention forms the cross-linked dispersant coating on the surface of the pigment particle, and even if the storage temperature is increased, the thermal motion of the dispersant coating with the cross-linked structure is low, and the coating of the pigment particle cannot be weakened.
The invention also aims to provide the aqueous pigment dispersion which has the characteristics of good dispersion effect and good storage stability.
It is a further object of the present invention to provide the use of an aqueous pigment dispersion having a better application effect in aqueous inks.
The technical scheme of the invention is as follows:
the preparation method of the aqueous pigment dispersion comprises the following steps of (by weight parts) raw materials of 20-50 parts of pigment, 2-10 parts of anionic polymerizable emulsifier, 3-25 parts of maleic acid monoalkyl ester polyether, 2-10 parts of hydrophobic monofunctional polymerizable monomer, 1-5 parts of hydrophobic polyfunctional polymerizable monomer, 0.05-0.5 part of oil-soluble azo free radical initiator, a proper amount of pH regulator and 50-100 parts of deionized water;
the preparation method comprises the following steps of grinding the pigment, the anionic polymerizable emulsifier, the monoalkyl maleate polyether, the hydrophobic monofunctional polymerizable monomer and the hydrophobic polyfunctional polymerizable monomer in a grinding machine for 3 times, adding the azo free radical initiator, uniformly stirring, dropwise adding the deionized water under high-speed stirring at the rotating speed of 800-2000rpm, adjusting the rotating speed to 200-300rpm, heating to 50-60 ℃ for reaction for 2-3 hours, heating to 60-80 ℃ for reaction for 3-5 hours, cooling, adding the pH regulator for adjusting the pH to 8-9, and thus obtaining the pigment.
Preferably, the pigment is selected from at least one of inorganic pigments and organic pigments. Specifically, the pigment may be a white pigment, such as titanium dioxide, zinc oxide, lithopone, or a yellow pigment, such as lead chrome yellow, iron yellow, lead silicochromate, strontium calcium yellow, transparent yellow, benzidine yellow, hansa yellow, or lemon yellow, or a red pigment, such as iron red, scarlet powder, chrome red, or transparent red, or a blue pigment, such as phthalocyanine blue, ultramarine, or a black pigment, such as carbon black, iron black, aniline black, or the like.
Preferably, the anionic polymerizable emulsifier is selected from at least one of 4-vinylbenzene sulfonate, allyl alkyl succinate sulfonate, maleic acid monoalkyl ester sulfonate, polyether maleate sulfonate, α -vinylphenoxy dodecyl sulfonate, acrylamide alkyl sulfonate, and acrylamide alkyl carboxylate.
The chemical general formula of the allyl alkyl succinic acid sulfonate is CH 2 ＝CHCH 2 OCOCH(SO 3 - M 1 + )CH 2 COO(CH 2 ) a CH 3 Wherein a > 11, M 1 + Is sodium ion or potassium ion.
The chemical general formula of the maleic acid monoalkyl ester sulfonate is CH 3 (CH 2 ) b OCOCH＝CHCOO(CH 2 ) 3 SO 3 - M 2 + Wherein b > 6,M 2 + Is sodium ion or potassium ion.
The chemical formula of the polyether maleate sulfonate is R 5 (OCH 2 CH 2 ) c OCOCH＝CHCOO(CH 2 ) 11 SO 3 - M 3 + Wherein c is more than or equal to 12 and less than or equal to 18 5 Independently selected from hydrogen, methyl, isobutyl or n-octyl, M 3 + Is sodium ion or potassium ion.
The chemical formula of the acrylamide alkyl sulfonate is CH 2 ＝CHCONHCH(CH 2 SO 3 - M 4 + )(CH 2 ) d CH 3 ，d＞7，M 4 + Is sodium ion or potassium ion.
Acrylamide alkyl carboxylate of the formula CH 3 (CH 2 ) 8 CH(NHCOCH＝CH 2 )(CH 2 ) 7 COO - M 5 + ，M 5 + Is sodium ion or potassium ion.
Preferably, the maleic acid monoalkyl ester polyether has a chemical formula of R 1 OOCCH＝CHCOO(CH 2 CH 2 O) n (CH 2 CHCH 3 O) m R 2 Wherein R is 1 Is C1-C7 alkyl, R 2 Independently selected from hydrogen, methyl, isobutyl or n-octyl, n is more than or equal to 5 and less than or equal to 40,0 and less than or equal to 30, and n-m is more than or equal to 8.
Preferably, the hydrophobic monofunctional polymerizable monomer may be selected from the group consisting of styrene, alpha-methylstyrene, tetrahydrofurfuryl (meth) acrylate, 2-phenoxyethyl acrylate, isobornyl (meth) acrylate, cyclobutyl (meth) acrylate, cyclopentyl (meth) acrylate, cyclohexyl (meth) acrylate, and the compound having the formula CH 2 ＝C(R 3 )COOR 4 At least one of (meth) acrylic acid esters of (a), wherein R 3 Independently selected from hydrogen or methyl, R 4 Is C1-C18 alkyl.
Preferably, the hydrophobic polyfunctional polymerizable monomer is selected from at least one of divinylbenzene, trivinylbenzene, tripropylene glycol diacrylate, dipentaerythritol hexaacrylate, hexanediol diacrylate, diethylene glycol diacrylate phthalate, neopentyl glycol diacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate, dipropylene glycol diacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, and 1,3-butanediol diacrylate.
Preferably, the oil-soluble azo-based radical initiator is at least one selected from the group consisting of azobisisobutyronitrile, azobisisovaleronitrile, dimethyl azobisisobutyrate, and azobisisoheptonitrile.
Preferably, the pH adjuster is an alkaline substance selected from at least one of ammonia, trimethylamine, triethanolamine, sodium bicarbonate, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium bicarbonate, diethanolamine, N-methyldiethanolamine, N-dimethyldiethanolamine, triethylamine, tributylamine, and N, N-dimethylaniline.
An aqueous pigment dispersion prepared by the method of any one of the above embodiments.
Use of an aqueous pigment dispersion according to one of the above embodiments in an aqueous ink.
The invention has the beneficial effects that:
(1) The preparation method of the aqueous pigment dispersion is a one-pot method, namely the preparation of the dispersing agent and the dispersing treatment of the dispersing agent on the pigment are carried out in one reaction kettle, and compared with the prior method of preparing the dispersing agent and then preparing the aqueous pigment dispersion by the dispersing agent, the preparation method of the aqueous pigment dispersion has the characteristics of reducing the process steps, improving the production efficiency and reducing the production cost.
Meanwhile, the method for preparing the dispersant in the prior art needs to use an organic solvent as a reaction solvent, and needs to remove the organic solvent subsequently, which has adverse effects on environment, safety, health of operators and cost. The preparation process is carried out in a water-based system, and the method has the advantages of high safety, low cost and environmental friendliness.
(2) The dispersant of the invention forms a coating layer with a cross-linked structure on the surface of the pigment, and the coating layer is provided with nonionic and anionic groups which can respectively form a steric hindrance effect and an electrostatic repulsion effect on the surface of the coating layer, so that the dispersant has good dispersion stability; the cross-linked structure of the coating layer improves the stability of the coating layer for coating the pigment, and even if the storage environment temperature of the aqueous pigment dispersion is increased, the coating is also stable and the effect is better.
(3) The prepared water-based pigment dispersoid has the characteristics of higher pigment content and good storage stability, and has good application effect in water-based ink.
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Unless otherwise specified, the parts in the following embodiments are parts by weight.
Example 1
The raw material formula comprises 24 parts of titanium dioxide, 3 parts of maleic acid monoalkyl ester sulfonate sodium and 12 parts of structural formula C 6 H 13 OOCCH＝CHCOO(CH 2 CH 2 O) 13.2 (CH 2 CHCH 3 O) 3.6 CH 3 4 parts of butyl acrylate, 1.3 parts of hexanediol diacrylate, 0.1 part of pentaerythritol tetraacrylate, 0.2 part of azobisisobutyronitrile, a proper amount of triethanolamine and 55 parts of deionized water;
grinding titanium dioxide, sodium maleic acid monoalkyl ester sulfonate, maleic acid monoalkyl ester polyether, butyl acrylate, pentaerythritol tetraacrylate and hexanediol diacrylate in a grinder for 3 times, adding azobisisobutyronitrile, uniformly stirring, dropwise adding deionized water under high-speed stirring at the rotating speed of 800-2000rpm, adjusting the rotating speed to 200-300rpm, heating to 60 ℃ for reaction for 2.5 hours, heating to 70 ℃ for reaction for 3-54 hours, cooling, adding triethanolamine to adjust the pH value to 8.0-8.5, and obtaining the water-based pigment dispersoid 1.
Example 2
The raw material formula comprises 32 parts of phthalocyanine blue, 5 parts of maleic acid monoalkyl ester sulfonate sodium and 5 parts of structural formula C 6 H 13 OOCCH＝CHCOO(CH 2 CH 2 O) 13.2 (CH 2 CHCH 3 O) 3.6 CH 3 Maleic acid monoalkyl ester polyether, 2 parts of butyl acrylate, 3 parts of styrene, 3 parts of divinylbenzene, 0.1 part of pentaerythritol tetraacrylate, 0.25 part of azobisisobutyronitrile, a proper amount of triethanolamine and 70 parts of deionized water;
grinding phthalocyanine blue, sodium maleic acid monoalkyl ester sulfonate, maleic acid monoalkyl ester polyether, butyl acrylate, styrene, pentaerythritol tetraacrylate and divinylbenzene in a grinding machine for 3 times, adding azodiisobutyronitrile, uniformly stirring, dropwise adding deionized water under high-speed stirring at the rotating speed of 1300rpm, adjusting the rotating speed to 200-300rpm, heating to 58 ℃ for reaction for 3 hours, heating to 75 ℃ for reaction for 3.5 hours, cooling, adding triethanolamine to adjust the pH value to 8.0-5.5, and obtaining the water-based pigment dispersoid 2.
Example 3
The raw material formula comprises 45 parts of carbon black, 7 parts of 4-vinyl benzene sodium sulfonate, 3 parts of acrylamide alkyl sodium sulfonate and 20 parts of structural formula C 6 H 13 OOCCH＝CHCOO(CH 2 CH 2 O) 15.2 (CH 2 CHCH 3 O) 4.1 CH 3 Maleic acid monoalkyl ester polyether, 7 parts of ethyl acrylate, 4 parts of divinylbenzene, 0.1 part of trivinylbenzene, 0.3 part of azobisisoheptonitrile, a proper amount of diethanolamine and 80 parts of deionized water;
grinding carbon black, 4-vinyl benzene sulfonic acid sodium salt, acrylamide alkyl sulfonic acid sodium salt, maleic acid monoalkyl ester polyether, ethyl acrylate, divinyl benzene and trivinyl benzene in a grinding machine for 3 times, adding azodiisoheptanonitrile, uniformly stirring, dropwise adding deionized water under high-speed stirring at the rotating speed of 1500rpm, adjusting the rotating speed to 200-300rpm, heating to 50 ℃ for reaction for 3 hours, heating to 70 ℃ for reaction for 3 hours, cooling, adding diethanol amine to adjust the pH value to 8.5-9.0, and preparing the aqueous pigment dispersoid 3.
Example 4
The raw material formula comprises 30 parts of transparent red, 3 parts of maleic acid monoalkyl ester sulfonate sodium, 1 part of 4-vinyl benzene sodium sulfonate and 8 parts of structural formula C 6 H 13 OOCCH＝CHCOO(CH 2 CH 2 O) 15. 2(CH 2 CHCH 3 O) 4.1 CH 3 3 parts of ethyl acrylate, 3 parts of hexanediol diacrylate, 0.1 part of trivinylbenzene, 0.3 part of azobisisoheptonitrile, a proper amount of triethylamine and 60 parts of deionized water;
grinding transparent red, maleic acid monoalkyl ester sulfonate sodium, 4-vinyl benzene sodium sulfonate, maleic acid monoalkyl ester polyether, ethyl acrylate, hexanediol diacrylate and trivinylbenzene in a grinding machine for 3 times, adding azobisisoheptonitrile, stirring uniformly, dropwise adding deionized water under high-speed stirring at the rotation speed of 900rpm, adjusting the rotation speed to 200-300rpm, heating to 52 ℃ for reaction for 3 hours, heating to 68 ℃ for reaction for 4 hours, cooling, adding triethylamine, adjusting the pH to 8.0-8.5, and preparing the aqueous pigment dispersoid 4.
Example 5
The transparent red in example 4 was changed to transparent yellow, and the other raw materials and preparation methods were the same as those in example 4.
Comparative example 1
The water-based pigment dispersion 5 is prepared by adopting a dispersant produced in a certain country to disperse carbon black according to a basic formula of 45 parts of carbon black, 45 parts of dispersant and 80 parts of deionized water.
Comparative example 2
The water-based pigment dispersion 6 is prepared by adopting a dispersant produced in a certain country to disperse transparent red and preparing the water-based pigment dispersion according to a basic formula of 30 parts of transparent red, 12 parts of dispersant and 60 parts of deionized water.
Comparative example 3
An imported dispersant is used to disperse carbon black and the basic formula of 45 parts of carbon black, 45 parts of dispersant and 80 parts of deionized water is used to prepare the aqueous pigment dispersion 7.
Comparative example 4
Transparent red is dispersed by adopting an imported dispersing agent, and the basic formula of 30 parts of transparent red, 12 parts of dispersing agent and 60 parts of deionized water is adopted for preparation, so that the water-based pigment dispersion 8 is obtained.
Test and results
(1) Viscosity of aqueous pigment dispersion: the aqueous pigment dispersions 1 to 8 were tested at 23 ℃ using a rotational viscometer, 20 rpm. The results are shown in Table 1.
(2) Storage stability: the aqueous pigment dispersions 1 to 8 were stored at 60 ℃ for 1 week, respectively, and it was observed whether or not precipitation and delamination occurred. The results are shown in Table 1.
(3) Cold-hot cycle stability: the aqueous pigment dispersions 1 to 8 are respectively kept stand at 70 ℃ for 4 hours, then kept at-20 ℃ for 4 hours, and circulated for 4 times. The change in particle size of the pigment particles before and after storage was measured using a laser particle sizer. The results are shown in Table 1.
(4) Compatibility: respectively and uniformly mixing the aqueous pigment dispersoid 1-8 with the single-component polyurethane white surface slurry according to the weight ratio of 3: 100, coating, and observing whether a paint film has floating color, flocculation or surface defects after drying. The results are shown in Table 1.
TABLE 1
The results in Table 1 show that the aqueous pigment dispersion obtained by the preparation method of the aqueous pigment dispersion has good dispersion effect, good dispersion stability, good storage property, good cold-resistant special cycle stability and good compatibility with polyurethane.
The foregoing has shown and described the principles, major features, and advantages of the invention. It should be understood by those skilled in the art that the present invention is not limited by the foregoing embodiments, which are merely preferred embodiments of the present invention, and the scope of the present invention should not be limited thereby, and that equivalent changes and modifications made within the scope of the present invention and the specification should be covered thereby. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. A method of preparing an aqueous pigment dispersion, characterized by: the raw materials comprise, by weight, 20-50 parts of pigment, 2-10 parts of anionic polymerizable emulsifier, 3-25 parts of maleic acid monoalkyl ester polyether, 2-10 parts of hydrophobic monofunctional polymerizable monomer, 1-5 parts of hydrophobic polyfunctional polymerizable monomer, 0.05-0.5 part of oil-soluble azo free radical initiator, a proper amount of pH regulator and 50-100 parts of deionized water;
the preparation method comprises the following steps of grinding the pigment, the anionic polymerizable emulsifier, the monoalkyl maleate polyether, the hydrophobic monofunctional polymerizable monomer and the hydrophobic polyfunctional polymerizable monomer in a grinding machine for 3 times, adding the azo free radical initiator, uniformly stirring, dropwise adding the deionized water under high-speed stirring at the rotating speed of 800-2000rpm, adjusting the rotating speed to 200-300rpm, heating to 50-60 ℃ for reaction for 2-3 hours, heating to 60-80 ℃ for reaction for 3-5 hours, cooling, adding the pH regulator for adjusting the pH to 8.0-9.0, and thus obtaining the pigment.
2. The method of claim 1, wherein: the pigment is selected from at least one of inorganic pigments and organic pigments.
3. The production method according to claim 1, characterized in that: the anionic polymerizable emulsifier is selected from at least one of 4-vinylbenzene sulfonate, allyl alkyl succinic acid sulfonate, maleic acid monoalkyl ester sulfonate, polyether maleic acid ester sulfonate, alpha-vinylphenoxy alkyl sulfonate, acrylamide alkyl sulfonate and acrylamide alkyl carboxylate.
4. The method of claim 1, wherein: the maleic acid monoalkylThe chemical formula of the polyether ester is R 1 OOCCH＝CHCOO(CH 2 CH 2 O) n (CH 2 CHCH 3 O) m R 2 Wherein R is 1 Is C1-C7 alkyl, R 2 Independently selected from hydrogen, methyl, isobutyl or n-octyl, n is more than or equal to 5 and less than or equal to 40,0 and less than or equal to 30, and n-m is more than or equal to 8.
5. The method of claim 1, wherein: the hydrophobic monofunctional polymerizable monomer may be selected from styrene, alpha-methylstyrene, tetrahydrofurfuryl (meth) acrylate, 2-phenoxyethyl acrylate, isobornyl (meth) acrylate, cyclobutyl (meth) acrylate, cyclopentyl (meth) acrylate, cyclohexyl (meth) acrylate and the general chemical formula CH 2 ＝C(R 3 )COOR 4 At least one of (meth) acrylic acid esters of (a), wherein R 3 Independently selected from hydrogen or methyl, R 4 Is C1-C18 alkyl.
6. The method of claim 1, wherein: the hydrophobic polyfunctional polymerizable monomer is selected from at least one of divinylbenzene, trivinylbenzene, tripropylene glycol diacrylate, dipentaerythritol hexaacrylate, hexanediol diacrylate, diethylene glycol diacrylate phthalate, neopentyl glycol diacrylate, pentaerythritol triacrylate, trimethylolpropane triacrylate, dipropylene glycol diacrylate, pentaerythritol tetraacrylate, dipentaerythritol pentaacrylate, and 1,3-butanediol diacrylate.
7. The method of claim 1, wherein: the oil-soluble azo free radical initiator is at least one selected from azobisisobutyronitrile, azobisisovaleronitrile, dimethyl azobisisobutyrate and azobisisoheptonitrile.
8. The production method according to claim 1, characterized in that: the pH regulator is an alkaline substance and is at least one selected from ammonia, trimethylamine, triethanolamine, sodium bicarbonate, sodium hydroxide, potassium hydroxide, sodium carbonate, potassium bicarbonate, diethanolamine, N-methyldiethanolamine, N-dimethyldiethanolamine, triethylamine, tributylamine and N, N-dimethylaniline.
9. An aqueous pigment dispersion prepared by the preparation method according to any one of claims 1 to 8.
10. Use of the aqueous pigment dispersion according to claim 9 in an aqueous ink.
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| US7205341B2 (en) * | 2002-08-29 | 2007-04-17 | Toyo Ink Mfg. Co., Ltd. | Aqueous pigment dispersion, inkjet ink, and process for producing aqueous pigment dispersion |
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