CN108047810B - Grain size control agent for wrapping red ink and yellow ink, and preparation method and application method thereof - Google Patents

Grain size control agent for wrapping red ink and yellow ink, and preparation method and application method thereof Download PDF

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CN108047810B
CN108047810B CN201711351742.9A CN201711351742A CN108047810B CN 108047810 B CN108047810 B CN 108047810B CN 201711351742 A CN201711351742 A CN 201711351742A CN 108047810 B CN108047810 B CN 108047810B
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吴爱勇
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Foshan Ngy Colour Co ltd
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09D11/02Printing inks
    • C09D11/03Printing inks characterised by features other than the chemical nature of the binder
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    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
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    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/58Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine
    • C08F220/585Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide containing oxygen in addition to the carbonamido oxygen, e.g. N-methylolacrylamide, N-(meth)acryloylmorpholine and containing other heteroatoms, e.g. 2-acrylamido-2-methylpropane sulfonic acid [AMPS]
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    • C09D11/00Inks
    • C09D11/02Printing inks
    • C09D11/10Printing inks based on artificial resins
    • C09D11/106Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C09D11/107Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof

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Abstract

The invention discloses a particle size control agent for wrapping red and yellow ink, a preparation method and an application method thereof, and the particle size control agent comprises the following raw material components in percentage by weight: 3-6% of 2-acrylamide-2-methylpropanesulfonic acid, 61-80% of methyl methacrylate, 15-31% of butyl acrylate and 2-5% of azobisisobutyronitrile. The zirconium silicate coated cadmium sulfoselenide coated ink has the advantages that the zirconium silicate coated cadmium sulfoselenide coated ink is convenient to use and good in storage stability, primary particles of a coated ink precursor synthesized by using the zirconium silicate coated cadmium sulfoselenide coated ink have the particle size of less than 100nm, the primary particles cannot be damaged through later grinding and subsequent treatment, the dispersed average particle size of the coated ink is 100nm, and the defect that the coloring power is reduced due to the fact that coated red and yellow pigments are ground too finely in the current market is overcome.

Description

Grain size control agent for wrapping red ink and yellow ink, and preparation method and application method thereof
Technical Field
The invention relates to the technical field of ink auxiliaries, in particular to a particle size control agent for wrapping red ink and yellow ink, a preparation method and an application method thereof.
Background
ZrSiO4 has high melting point (2500 ℃), high refractive index (1.93-2.01) and the characteristic of high-temperature resistant glaze melt, so that the ZrSiO4 becomes a preferred wrapping phase for wrapping scarlet and yellow, causes wide attention of scholars at home and abroad, and develops a batch of products wrapping red and yellow ceramic printing ink.
In the prior art, the synthesis method of zirconium silicate coated red-yellow pigments is related, but the average particle size of the coated red-yellow pigments synthesized by the method is more than 0.6um, so that the particles with the size are easy to agglomerate in aqueous solution, and are easy to precipitate, and the method cannot be used for preparing stable ceramic ink. In order to meet the use requirements of ink for ink-jet printing, the pigment with coarse particles needs to be ground, and the color development performance of the pigment is poor due to the reduction of chroma after grinding and the damage of the crystal structure of the pigment. The reason for this is that finer grinding of the pigment will destroy the already coated structure, lose its high temperature stability, turn white after firing and fade extremely severely.
Therefore, the synthesis process of the encapsulated red and yellow pigments needs to be controlled at a nanometer level, and a post-grinding method cannot be relied on, which is a great problem in the synthesis of the current encapsulated red and yellow ink.
Disclosure of Invention
In view of the above, the invention provides a particle size control agent for coating red and yellow ink, a preparation method and an application method thereof.
A particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000011
Figure BDA0001510392370000021
preferably, the raw material components by weight percentage are as follows:
Figure BDA0001510392370000022
preferably, the mass ratio of methyl methacrylate to butyl acrylate is 2-5: 1.
A preparation method of a particle size control agent for wrapping red and yellow ink comprises the following steps:
carrying out reduced pressure distillation pretreatment on methyl methacrylate and butyl acrylate, wherein the distillation temperatures are respectively 40 ℃ and 60 ℃ under 10.8 kPa;
putting 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate and butyl acrylate into a mixed solvent of N-N dimethylformamide and isopropanol to be fully dissolved for later use;
and fully and uniformly mixing the dissolved 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate and butyl acrylate, dropwise adding azodiisobutyronitrile by using a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, continuously dropwise adding, and finishing dropwise adding within 0.5-6 hours to obtain the coarse control preparation.
Preferably, the method further comprises:
adding the obtained control agent into acetone, and performing extraction separation and purification to obtain an extract liquid;
and (3) putting the extract liquor into a drying box, drying at a constant temperature of 313k, and drying the extract liquor to obtain the special particle size control agent for the red and yellow coated ceramic ink.
Preferably, the input amount ratio of the methyl methacrylate to the butyl acrylate is 2-5: 1.
A method for applying a particle size control agent for coating red and yellow ink comprises the following steps:
in the preparation process of the precursor wrapped with the red and yellow ceramic inks, the particle size control agent is directly added, and the addition amount is 2-20% of the weight percentage of the synthetic precursor.
Preferably, the addition amount of the particle size control agent is 5-10% of the weight percentage of the synthetic precursor.
The particle size control agent zirconium silicate is used for wrapping cadmium sulfoselenide in the wrapping ink, the use is convenient, the storage stability is good, the particle size of primary particles of a wrapping ink precursor synthesized by using the particle control agent reaches below 100nm, the primary particles cannot be damaged after post-grinding subsequent treatment, the average dispersed particle size of the wrapping ink is 100nm, and the defect that the coloring power is reduced due to the fact that the red and yellow pigment wrapping material is ground too finely at present on the market is overcome. The coating method essentially overcomes the defects of large red and yellow ink coating particles and poor dispersibility, and has great market prospect. The added particle control agent can reduce the activation energy generated by cadmium sulfoselenide hydrosol and the particle size of the cadmium sulfoselenide sol, the primary particle size is less than 50nm, the generated composite anchoring group can directionally adsorb Si-OH bonds and Zr-OH bonds of silicon dioxide, so that the silicon dioxide can be tightly combined with the generated cadmium sulfoselenide colloidal particles to form a firm zirconium silicate coated cadmium sulfoselenide structural unit, and the formed structural unit is less than 100nm and far less than the particle size of particles coated with red yellow ink on the market.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is apparent that the drawings in the following description are some embodiments of the present invention.
FIG. 1 is a TEM image of primary particles of cadmium sulfoselenide sol;
FIG. 2 is a TEM image of a coated red-yellow ceramic printing ink synthesized by the particle size control agent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It should be further understood that the term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.
Example 1
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000041
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
in the preparation process of a precursor for wrapping scarlet ceramic ink in zirconium silicate wrapped cadmium sulfoselenide wrapping ink, the particle size control agent is directly added, the addition amount is 6 wt% of the synthetic precursor, and the ceramic ink is obtained.
Example 2
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000051
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
and in the preparation process of the precursor wrapping the yellow ceramic ink, directly adding the particle size control agent, wherein the addition amount is 8 wt% of the synthetic precursor, and obtaining the ceramic ink.
Example 3
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000061
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
in the preparation process of the precursor wrapping the scarlet ceramic ink, the particle size control agent is directly added, and the addition amount is 2 wt% of the synthetic precursor, so that the ceramic ink is obtained.
Example 4
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000071
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
and in the preparation process of the precursor wrapping the yellow ceramic ink, directly adding the particle size control agent, wherein the addition amount is 20 wt% of the synthetic precursor, and obtaining the ceramic ink.
Example 5
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000081
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
and in the preparation process of the precursor wrapping the scarlet ceramic ink, directly adding the particle size control agent, wherein the addition amount is 5 wt% of the synthetic precursor, and obtaining the ceramic ink.
Example 6
The particle size control agent for wrapping red and yellow ink comprises the following raw material components in percentage by weight:
Figure BDA0001510392370000091
the preparation method comprises the following steps:
accurately weighing 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate, butyl acrylate and azobisisobutyronitrile in component parts;
carrying out reduced pressure distillation pretreatment on Methyl Methacrylate (MMA) and Butyl Acrylate (BA) at the distillation temperatures of 40 ℃ and 60 ℃ respectively under 10.8 kPa;
adding 2-acrylamide-2-methylpropanesulfonic Acid (AMPS), MMA and BA in component amount into a mixed solvent of N-N Dimethylformamide (DMF) and isopropanol, and dissolving for later use;
the reactants are fully and uniformly mixed, Azodiisobutyronitrile (AIBN) is dripped by a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, and the dripping is continuously carried out for 0.5-6 hours;
and after the reaction is finished, extracting, separating and purifying the reaction mixed solution by using acetone, and drying the obtained solution in a constant-temperature drying box under 313K to obtain the special particle size control agent for the red and yellow coated ceramic ink.
The application method comprises the following steps:
and in the preparation process of the precursor wrapping the yellow ceramic ink, directly adding the particle size control agent, wherein the addition amount is 10 wt% of the synthetic precursor, and obtaining the ceramic ink.
Comparative example 1
And in the preparation process of the precursor wrapping the scarlet ceramic ink, the particle size control agent is not added to obtain the ceramic ink.
Comparative example 2
And in the preparation process of the precursor wrapping the yellow ceramic ink, the ceramic ink is obtained without adding the particle size control agent.
The coated red-yellow ceramic printing inks of examples 1-6 were physico-chemically characterized as compared to comparative examples 1-2, with the following results:
Figure BDA0001510392370000101
Figure BDA0001510392370000111
from the data in the table, in conjunction with the TEM images of fig. 1 and 2, it can be seen that: the synthesized particle control agent is used in the coating ink of zirconium silicate coated cadmium sulfoselenide, is convenient to use and good in storage stability, the particle size of primary particles of a precursor of the coating ink synthesized by using the particle control agent reaches about 100nm, more preferably below 100nm, the primary particles cannot be damaged through post-grinding subsequent treatment, the dispersed average particle size of the coating ink is 100nm, the defect that the coloring power is reduced due to the fact that the red and yellow pigment coated on the market is ground too finely is overcome, and the particle control agent has a great market prospect. The defects of large red and yellow ink coating particles and poor dispersibility are essentially overcome, and the method has great market prospect. The added particle control agent can reduce the activation energy generated by cadmium sulfoselenide hydrosol and the particle size of the cadmium sulfoselenide sol, the primary particle size is less than 50nm, the generated composite anchoring group can directionally adsorb Si-OH bonds and Zr-OH bonds of silicon dioxide, so that the silicon dioxide can be tightly combined with the generated cadmium sulfoselenide colloidal particles to form a firm zirconium silicate coated cadmium sulfoselenide structural unit, and the formed structural unit is less than 100nm and far less than the particle size of particles coated with red yellow ink on the market.
The steps in the method of the embodiment of the invention can be sequentially adjusted, combined and deleted according to actual needs.
The present invention has been described in detail, and the principle and embodiments of the present invention are explained by applying specific examples, which are only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.

Claims (2)

1. An application method of a particle size control agent for wrapping red and yellow ink is characterized in that the particle size control agent is directly added in the preparation process of a precursor wrapping the red and yellow ceramic ink, and the addition amount of the particle size control agent is 2-20% of the weight percentage of the synthetic precursor;
the particle size control agent comprises the following raw material components in percentage by weight:
Figure FDA0002732207100000011
the preparation method of the particle size control agent comprises the following steps:
carrying out reduced pressure distillation pretreatment on methyl methacrylate and butyl acrylate, wherein the distillation temperatures are respectively 40 ℃ and 60 ℃ under 10.8 kPa;
putting 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate and butyl acrylate into a mixed solvent of N-N dimethylformamide and isopropanol to be fully dissolved for later use;
fully and uniformly mixing the dissolved 2-acrylamide-2-methylpropanesulfonic acid, methyl methacrylate and butyl acrylate, dropwise adding azodiisobutyronitrile by using a constant flow pump at the stirring speed of 180r/min and the temperature of 40-80 ℃, continuously dropwise adding, and finishing dropwise adding within 0.5-6 hours to obtain a coarse control preparation;
adding the obtained crude control preparation into acetone, and performing extraction, separation and purification to obtain an extract liquid;
and (3) putting the extract liquor into a drying box, drying at a constant temperature of 313k, and drying the extract liquor to obtain the special particle size control agent for the red and yellow coated ceramic ink.
2. The method of application of claim 1, wherein: the addition amount of the particle size control agent is 5-10% of the weight percentage of the synthetic precursor.
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WO2016011277A1 (en) * 2014-07-16 2016-01-21 Electronics For Imaging, Inc. Ceramic inkjet ink for red decoration
CN106590031A (en) * 2016-12-02 2017-04-26 佛山市华意陶瓷颜料有限公司 Cadmium sulfoselenide occlusion pigment, ceramic ink and preparation method of cadmium sulfoselenide occlusion pigment
CN106752108A (en) * 2016-12-02 2017-05-31 佛山市华意陶瓷颜料有限公司 A kind of yellow cadmium system occlusion pigment, ceramic ink and preparation method thereof

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CN103224727A (en) * 2013-04-08 2013-07-31 佛山市道氏科技有限公司 Eco-friendly glaze ink for ceramic jet printing and preparation method thereof
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