CN107151293A - A kind of aqueous effect pigment of amide modifications aligns agent and preparation method thereof - Google Patents
A kind of aqueous effect pigment of amide modifications aligns agent and preparation method thereof Download PDFInfo
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- CN107151293A CN107151293A CN201710271529.0A CN201710271529A CN107151293A CN 107151293 A CN107151293 A CN 107151293A CN 201710271529 A CN201710271529 A CN 201710271529A CN 107151293 A CN107151293 A CN 107151293A
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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
- C08F283/04—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides
- C08F283/045—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polycarbonamides, polyesteramides or polyimides on to unsaturated polycarbonamides, polyesteramides or polyimides
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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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
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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
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
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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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/26—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids
- C08G69/34—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from polyamines and polycarboxylic acids using polymerised unsaturated fatty acids
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Abstract
The present invention relates to coating additive technical field, and in particular to a kind of aqueous effect pigment of amide modifications aligns agent and preparation method thereof, and the aqueous effect pigment of the amide modifications aligns agent and is made up of the raw material of following parts by weight：50 150 parts of 35 parts of organic diamine, 5 25 parts of unsaturated dibasic acid, 10 50 parts of monomer, 1 10 parts of emulsifying agent, 35 parts of nertralizer, 0.5 5 parts of initiator and deionized water.It is zero that the aqueous effect pigment of amide modifications of the present invention, which aligns agent VOC emission, due to introducing amide group, bonding ability is stronger, thixotropy is also more preferable, aligning property and metal sense are stronger, and application field is wider, particularly to there is the water-based system of cosolvent, though polarity height or addition number, can be applicable.
Description
Technical field
The present invention relates to coating additive technical field, and in particular to a kind of aqueous effect pigment of amide modifications aligns agent
And preparation method thereof.
Background technology
In face of the environment gone from bad to worse, countries in the world are deeply concerned to the height of environmental protection, and external latter stage in 20th century begins to
Carry out the low VOC content even exploitation of the coating and printing ink of Diamond Search content, using water paint, ink substitute existing technique and
Petroleum solvent coating, the ink of technology maturation are trends of the times.
Due to fashion, the demand driving of automobile and other consumption markets can produce the pigment of special effects（Such as with angle
Heterochromatic effect or ornamental clour effect）, the economic value with growth and can be in various industrial products and terminal user
It is widely applied.In terms of decorative use, special effect pigment has following three kinds of advantages：（a）This pigment can be created
The illusion that the optics depth is not surveyed, such as using pearlescent pigment just it is observed that this phenomenon in Automobile Paints；（b）This pigment
The surprised color effect that unintelligible changeable colors along with angle attracts eyeball can be produced, such as available for Automobile Paints or ornamental color printing
In；（c）The effect that this pigment can simulate natural peral is applied in button, plastic bottle and a lot of other decorative articles.
The coating manufactured in solvent based coating ink using effect pigment has obtained everybody extensive approval, yet with not having
Pearlescent pigment, the aluminium powder pigment that aqueous effect pigment is aligned in agent, aqueous imitative metallic paint are desultorily distributed in painting
So as to have impact on the reflection of light in material so that metal sense declines, the metal sense for imitating metallic paint without solvent-borne type is good, so that
The application for influenceing aqueous imitative metallic paint to promote.
Although having the product of correlation abroad in sale, the also patent without this part, domestic patent
The arrangement agent that CN102344710A is prepared after being dissolved using solvent in the method emulsified, but still had in formula
VOC compositions；Prepared by CN105399883A to align agent more sensitive for the cosolvent of water-based system, when hydrotropy dosage
Occur that directional effect is bad or completely without directional effect when comparing many or when polarity is relatively low.
The content of the invention
In order to overcome shortcoming and defect present in prior art, it is an object of the invention to provide a kind of amide modifications water
Property effect pigment aligns agent, and it is zero that the aqueous effect pigment of the amide modifications, which aligns agent VOC emission, due to introducing acyl
Amine groups, bonding ability is stronger, and thixotropy is also more preferable, and aligning property and metal sense are stronger, and application field is wider, especially
To there is the water-based system of cosolvent, though polarity height or addition number, can be applicable.
The preparation method of agent is aligned another object of the present invention is to provide a kind of aqueous effect pigment of amide modifications, should
Preparation method step is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low, up to the production of technical scale metaplasia.
The purpose of the present invention is achieved through the following technical solutions：A kind of aqueous effect pigment of amide modifications aligns agent,
It is made up of the raw material of following parts by weight：
3-5 parts of organic diamine
5-25 parts of unsaturated dibasic acid
10-50 parts of monomer
1-10 parts of emulsifying agent
3-5 parts of nertralizer
0.5-5 parts of initiator
50-150 parts of deionized water.
It is preferred that, it is made up of the raw material of following parts by weight：
3-5 parts of organic diamine
5-20 parts of unsaturated dibasic acid
15-40 parts of monomer
2-8 parts of emulsifying agent
3-5 parts of nertralizer
1-5 parts of initiator
50-120 parts of deionized water.
It is preferred that, the organic diamine is at least one in ethylenediamine, propane diamine, butanediamine, hexamethylene diamine and polyether diamine
Kind.The present invention is by using above-mentioned organic diamine, and obtained to align that agent bonding ability is stronger, thixotropy is also more preferable, orientation
Arrangement property and metal sense are stronger.
It is preferred that, the unsaturated dibasic acid is in itaconic acid, fumaric acid, octadecene diacid and heptadecene diacid
It is at least one.The present invention is by using above-mentioned unsaturated dibasic acid, and the obtained agent bonding ability that aligns is stronger, thixotropy
More preferably, aligning property and metal sense are stronger.
It is preferred that, the monomer is acrylic monomers and/or methacrylic acid monomer.The present invention is by using above-mentioned list
Body, obtained to align that agent bonding ability is stronger, thixotropy is also more preferable, and aligning property and metal sense are stronger.
It is preferred that, the acrylic monomers is acrylic acid and/or acrylate.It is more highly preferred to, the acrylic monomers
2-4 is compared with weight for acrylic acid, butyl acrylate and vinylacetate：5-7：The mixture of 1 composition.The present invention is by using upper
State acrylic monomers, obtained to align that agent bonding ability is stronger, thixotropy is also more preferable, and aligning property and metal sense are more
By force.
It is preferred that, the methacrylic acid monomer is methacrylic acid and/or methacrylate.The methacrylic acid
The structural formula of ester is H2C=C(R)-CO-0-(CHZ-CH20)n-R0, wherein, R is H or CH3, n is 2-100 natural number, R0It is to contain
There are the group, the alkyl acrylate containing 4-11 carbon atom, the methyl-prop containing 5-12 carbon atom of 4-36 carbon atom
Olefin(e) acid Arrcostab, vinylacetate or styrene.The present invention is obtained to align by using above-mentioned methacrylic acid monomer
Agent bonding ability is stronger, and thixotropy is also more preferable, and aligning property and metal sense are stronger.
It is preferred that, the emulsifying agent is isomerous tridecanol polyoxyethylene ether, straight-chain fatty alcohol APEO, succinic acid sulphur
At least one of sour sodium, diisobutyl Cai sodium sulfonate, neopelex and lauryl sodium sulfate.The present invention passes through
Using mentioned emulsifier, its emulsifying effectiveness is good, is conducive to the progress of polymerisation.
It is preferred that, the nertralizer is 2-amino-2-methyl-1-propanol, the propyl alcohol of 2- amino -2- ethyls -1,3- bis-, Dan Yi
At least one of hydramine, dimethylethanolamine, butylethanolamine, butyl diethanolamine and aminopropyltriethoxy monoethanolamine.This hair
It is bright by using above-mentioned nertralizer, its neutralization is good.
It is preferred that, the initiator is at least one of potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate.The present invention passes through
Using above-mentioned initiator, it triggers effect good, can trigger radical polymerization and copolymerization, can improve the polymerization speed of monomer
Rate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 150-160 DEG C of dehydration
0.5-1h, is evacuated to 0.095MPa, keeps being cooled to 80-100 DEG C after 0.5-1h, adds nertralizer and neutralizes, adds and account for
Ion water inventory 10%-20% deionized water dissolving, be cooled to 30-40 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 50%-60%, after stirring,
Monomer emulsification 10-60min is added, pre-emulsion is obtained；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 5-20%, stirs, obtain
Initiator solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added for 5-30% pre-emulsion anti-
Answer in kettle, 75-85 DEG C is warming up under rotating speed 400-800RPM, addition mass percent is 3-8% initiator solutions, constant temperature is pre-
Poly- 0.5-1.5h, you can obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
1.5-4.0h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 2.0-4.5h at the uniform velocity completion of dropping, drop is added dropwise
Plus during keep rotating speed to be 400-800RPM, temperature is 75-85 DEG C, keeping temperature 75-85 after all materials completion of dropping
DEG C insulation 0.5-2.0h, then 80-95 DEG C of insulation 0.5-3.0h is warming up to, it is subsequently cooled to 20-40 DEG C, acyl is made in filtering and discharging
Amine modified water-soluble effect pigment aligns agent.
Intermediate is dissolved in by the present invention by will be neutralized after organic diamine and unsaturated dibasic acid reaction with nertralizer
As backing material in water, instilled with the monomer of emulsifier and pass through radical polymerization equipped with backing material, initiator, deionized water
Close, you can obtain the aqueous effect pigment of amide modifications and align agent.
The beneficial effects of the present invention are：The aqueous effect pigment of amide modifications of the present invention aligns agent VOC emission and is
Zero, due to introducing amide group, bonding ability is stronger, and thixotropy is also more preferable, and aligning property and metal sense are stronger, Er Qieying
It is wider with field, particularly to there is the water-based system of cosolvent, though polarity height or addition number, can fit
With.
The preparation method of agent is aligned another object of the present invention is to provide a kind of aqueous effect pigment of amide modifications,
The preparation method step is simple, convenient operation and control, steady quality, and production efficiency is high, and production cost is low, up to technical scale
Production.
Embodiment
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying is referred to not limitation of the invention.
Embodiment 1
A kind of aqueous effect pigment of amide modifications aligns agent, is made up of the raw material of following parts by weight：
3 parts of organic diamine
5 parts of unsaturated dibasic acid
10 parts of monomer
1 part of emulsifying agent
3 parts of nertralizer
0.5 part of initiator
50 parts of deionized water.
The organic diamine is ethylenediamine.
The unsaturated dibasic acid is itaconic acid.
The monomer is acrylic monomers.
The acrylic monomers is acrylic acid and/or acrylate.The acrylic monomers is acrylic acid, butyl acrylate
With vinylacetate with weight ratio 2：5：The mixture of 1 composition.
The emulsifying agent is isomerous tridecanol polyoxyethylene ether.
The nertralizer is 2-amino-2-methyl-1-propanol or the propyl alcohol of 2- amino -2- ethyls -1,3- bis-.
The initiator is potassium peroxydisulfate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 150 DEG C of dehydration 0.5h,
0.095MPa is evacuated to, keeps being cooled to 80 DEG C after 0.5h, nertralizer is added and neutralizes, add and account for ion water inventory 10%
Deionized water dissolving, be cooled to 30 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 50%, after stirring, added
Monomer emulsifies 10min, obtains pre-emulsion；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 5-20%, stirs, obtain
Initiator solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added into reactor for 5% pre-emulsion
In, 75 DEG C are warming up under rotating speed 400RPM, addition mass percent is 3-8% initiator solutions, constant temperature pre-polymerization 0.5h, you can
Obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
1.5h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 2.0h at the uniform velocity completion of dropping, during dropwise addition is added dropwise
Holding rotating speed is 400RPM, and temperature is 75 DEG C of insulation 0.5h of keeping temperature after 75 DEG C, all materials completion of dropping, then is warming up to
80 DEG C of insulation 0.5h, are subsequently cooled to 20 DEG C, filtering and discharging is made the aqueous effect pigment of amide modifications and aligns agent.
Embodiment 2
A kind of aqueous effect pigment of amide modifications aligns agent, is made up of the raw material of following parts by weight：
3 parts of organic diamine
5 parts of unsaturated dibasic acid
15 parts of monomer
2 parts of emulsifying agent
3 parts of nertralizer
1 part of initiator
50 parts of deionized water.
The organic diamine is propane diamine.
The unsaturated dibasic acid is fumaric acid.
The monomer is methacrylic acid monomer.
The methacrylic acid monomer is methacrylic acid and/or methacrylate.
The structural formula of the methacrylate is H2C=C(R)-CO-0-(CHZ-CH20)n-R0, wherein, R is H or CH3, n
For 20, R0It is the group containing 4-36 carbon atom.
The emulsifying agent is straight-chain fatty alcohol APEO.
The nertralizer is MEA.
The initiator is sodium peroxydisulfate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 152 DEG C of dehydration 0.6h,
0.095MPa is evacuated to, keeps being cooled to 85 DEG C after 0.6h, nertralizer is added and neutralizes, add and account for ion water inventory 12%
Deionized water dissolving, be cooled to 32 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 52%, after stirring, added
Monomer emulsifies 20min, obtains pre-emulsion；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 8%, stirred, must triggered
Agent solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added into reaction for 10% pre-emulsion
In kettle, 78 DEG C are warming up under rotating speed 500RPM, addition mass percent is 3-8% initiator solutions, constant temperature pre-polymerization 0.8h, i.e.,
It can obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion 2h are added dropwise into prepolymer
At the uniform velocity completion of dropping, while remaining initiator solution is added dropwise, initiator solution 2.5h at the uniform velocity completion of dropping is kept during dropwise addition
Rotating speed is 500RPM, and temperature is 78 DEG C of insulation 0.8h of keeping temperature after 78 DEG C, all materials completion of dropping, then is warming up to 84 DEG C
1h is incubated, 25 DEG C are subsequently cooled to, filtering and discharging is made the aqueous effect pigment of amide modifications and aligns agent.
Embodiment 3
A kind of aqueous effect pigment of amide modifications aligns agent, is made up of the raw material of following parts by weight：
4 parts of organic diamine
15 parts of unsaturated dibasic acid
30 parts of monomer
5 parts of emulsifying agent
4 parts of nertralizer
2.5 parts of initiator
100 parts of deionized water.
The organic diamine is butanediamine.
The unsaturated dibasic acid is octadecene diacid.
The monomer is acrylic monomers.
The acrylic monomers is acrylic acid and/or acrylate.The acrylic monomers is acrylic acid, butyl acrylate
With vinylacetate with weight ratio 3：6：The mixture of 1 composition.
The emulsifying agent is succinic acid sodium sulfonate.
The nertralizer is dimethylethanolamine.
The initiator is ammonium persulfate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 155 DEG C of dehydration 0.8h,
0.095MPa is evacuated to, keeps being cooled to 90 DEG C after 0.8h, nertralizer is added and neutralizes, add and account for ion water inventory 10%-
20% deionized water dissolving, be cooled to 35 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 55%, after stirring, added
Monomer emulsifies 35min, obtains pre-emulsion；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 12%, stirred, must drawn
Send out agent solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added into reaction for 20% pre-emulsion
In kettle, 80 DEG C are warming up under rotating speed 600RPM, addition mass percent is 3-8% initiator solutions, constant temperature pre-polymerization 1h, you can
Obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
2.5h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 3.5h at the uniform velocity completion of dropping, during dropwise addition is added dropwise
Holding rotating speed is 600RPM, and temperature is 80 DEG C of insulation 1.2h of keeping temperature after 80 DEG C, all materials completion of dropping, then is warming up to
88 DEG C of insulation 2h, are subsequently cooled to 30 DEG C, filtering and discharging is made the aqueous effect pigment of amide modifications and aligns agent.
Embodiment 4
A kind of aqueous effect pigment of amide modifications aligns agent, is made up of the raw material of following parts by weight：
3-5 parts of organic diamine
5-25 parts of unsaturated dibasic acid
10-50 parts of monomer
1-10 parts of emulsifying agent
3-5 parts of nertralizer
0.5-5 parts of initiator
50-150 parts of deionized water.
It is made up of the raw material of following parts by weight：
3-5 parts of organic diamine
5-20 parts of unsaturated dibasic acid
15-40 parts of monomer
2-8 parts of emulsifying agent
3-5 parts of nertralizer
1-5 parts of initiator
50-120 parts of deionized water.
The organic diamine is hexamethylene diamine.
The unsaturated dibasic acid is heptadecene diacid.
The monomer is methacrylic acid monomer.
The methacrylic acid monomer is methacrylic acid and/or methacrylate.
The structural formula of the methacrylate is H2C=C(R)-CO-0-(CHZ-CH20)n-R0, wherein, R is H or CH3, n
For 80, R0It is the alkyl acrylate containing 4-11 carbon atom, the alkyl methacrylate containing 5-12 carbon atom, vinegar
Vinyl acetate or styrene.
The emulsifying agent is diisobutyl Cai's sodium sulfonate.
The nertralizer is butylethanolamine or butyl diethanolamine.
The initiator is potassium peroxydisulfate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 150-160 DEG C of dehydration
0.5-1h, is evacuated to 0.095MPa, keeps being cooled to 80-100 DEG C after 0.5-1h, adds nertralizer and neutralizes, adds and account for
Ion water inventory 10%-20% deionized water dissolving, be cooled to 30-40 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 50%-60%, after stirring,
Monomer emulsification 10-60min is added, pre-emulsion is obtained；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 5-20%, stirs, obtain
Initiator solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added for 5-30% pre-emulsion anti-
Answer in kettle, 75-85 DEG C is warming up under rotating speed 400-800RPM, addition mass percent is 3-8% initiator solutions, constant temperature is pre-
Poly- 0.5-1.5h, you can obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
1.5-4.0h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 2.0-4.5h at the uniform velocity completion of dropping, drop is added dropwise
Plus during keep rotating speed to be 400-800RPM, temperature is 75-85 DEG C, keeping temperature 75-85 after all materials completion of dropping
DEG C insulation 0.5-2.0h, then 80-95 DEG C of insulation 0.5-3.0h is warming up to, it is subsequently cooled to 20-40 DEG C, acyl is made in filtering and discharging
Amine modified water-soluble effect pigment aligns agent.
Embodiment 5
A kind of aqueous effect pigment of amide modifications aligns agent, is made up of the raw material of following parts by weight：
5 parts of organic diamine
25 parts of unsaturated dibasic acid
50 parts of monomer
10 parts of emulsifying agent
5 parts of nertralizer
5 parts of initiator
150 parts of deionized water.
The organic diamine is polyether diamine.
The unsaturated dibasic acid is itaconic acid.
The monomer is acrylic monomers.
The acrylic monomers is acrylic acid and/or acrylate.The acrylic monomers is acrylic acid, butyl acrylate
With vinylacetate with weight ratio 4：7：The mixture of 1 composition.
The emulsifying agent is neopelex or lauryl sodium sulfate.
The nertralizer is aminopropyltriethoxy monoethanolamine.
The initiator is at least one of potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate.
A kind of aqueous effect pigment of amide modifications aligns the preparation method of agent, comprises the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 160 DEG C of dehydration 1h, are taken out
Vacuum keeps being cooled to 100 DEG C after 1h to 0.095MPa, adds nertralizer and neutralizes, adds and account for going for ion water inventory 20%
Ionized water dissolve, be cooled to 40 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 60%, after stirring, added
Monomer emulsifies 60min, obtains pre-emulsion；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 5-20%, stirs, obtain
Initiator solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added into reaction for 30% pre-emulsion
In kettle, 85 DEG C are warming up under rotating speed 800RPM, addition mass percent is 8% initiator solution, constant temperature pre-polymerization 1.5h, you can
Obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
4.0h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 4.5h at the uniform velocity completion of dropping, during dropwise addition is added dropwise
Holding rotating speed is 800RPM, and temperature is 85 DEG C of insulation 2.0h of keeping temperature after 85 DEG C, all materials completion of dropping, then is warming up to
95 DEG C of insulation 3.0h, are subsequently cooled to 40 DEG C, filtering and discharging is made the aqueous effect pigment of amide modifications and aligns agent.
Above-described embodiment is the present invention preferably implementation, and in addition, the present invention can be realized with other manner,
Any obvious replacement is within protection scope of the present invention on the premise of not departing from present inventive concept.
Claims (10)
1. a kind of aqueous effect pigment of amide modifications aligns agent, it is characterised in that：It is made up of the raw material of following parts by weight：
3-5 parts of organic diamine
5-25 parts of unsaturated dibasic acid
10-50 parts of monomer
1-10 parts of emulsifying agent
3-5 parts of nertralizer
0.5-5 parts of initiator
50-150 parts of deionized water.
2. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：By following
The raw material composition of parts by weight：
3-5 parts of organic diamine
5-20 parts of unsaturated dibasic acid
15-40 parts of monomer
2-8 parts of emulsifying agent
3-5 parts of nertralizer
1-5 parts of initiator
50-120 parts of deionized water.
3. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：It is described to have
Machine diamines is at least one of ethylenediamine, propane diamine, butanediamine, hexamethylene diamine and polyether diamine.
4. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：It is described not
Monounsaturated dicarboxylic acid is at least one of itaconic acid, fumaric acid, octadecene diacid and heptadecene diacid.
5. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：The list
Body is acrylic monomers and/or methacrylic acid monomer, and the acrylic monomers is acrylic acid and/or acrylate；The first
Base acrylic monomers is methacrylic acid and/or methacrylate.
6. the aqueous effect pigment of a kind of amide modifications according to claim 6 aligns agent, it is characterised in that：The first
The structural formula of base acrylate is H2C=C(R)-CO-0-(CHZ-CH20)n-R0, wherein, R is H or CH3, n is 2-100 nature
Number, R0It is the group containing 4-36 carbon atom, the alkyl acrylate containing 4-11 carbon atom, containing 5-12 carbon atom
Alkyl methacrylate, vinylacetate or styrene.
7. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：The breast
Agent is isomerous tridecanol polyoxyethylene ether, straight-chain fatty alcohol APEO, succinic acid sodium sulfonate, diisobutyl Cai's sulfonic acid
At least one of sodium, neopelex and lauryl sodium sulfate.
8. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：In described
It is 2-amino-2-methyl-1-propanol, the propyl alcohol of 2- amino -2- ethyls -1,3- bis-, MEA, dimethylethanolamine, fourth with agent
At least one of ethylethanolamine, butyl diethanolamine and aminopropyltriethoxy monoethanolamine.
9. the aqueous effect pigment of a kind of amide modifications according to claim 1 aligns agent, it is characterised in that：It is described to draw
Hair agent is at least one of potassium peroxydisulfate, sodium peroxydisulfate and ammonium persulfate.
10. the aqueous effect pigment of a kind of amide modifications as described in claim any one of 1-9 aligns the preparation method of agent,
It is characterized in that：Comprise the following steps：
（1）The preparation of intermediate：Organic diamine and unsaturated dibasic acid are added in a kettle., are warming up to 150-160 DEG C of dehydration
0.5-1h, is evacuated to 0.095MPa, keeps being cooled to 80-100 DEG C after 0.5-1h, adds nertralizer and neutralizes, adds and account for
Ion water inventory 10%-20% deionized water dissolving, be cooled to 30-40 DEG C it is stand-by；
（2）The preparation of pre-emulsion：Emulsifying agent is dissolved in the deionized water for accounting for ion water inventory 50%-60%, after stirring,
Monomer emulsification 10-60min is added, pre-emulsion is obtained；
The preparation of initiator solution：Initiator is dissolved in the deionized water for accounting for ion water inventory 5-20%, stirs, obtain
Initiator solution；
（3）The preparation of prepolymer：Intermediate, remaining deionized water and mass percent are added for 5-30% pre-emulsion anti-
Answer in kettle, 75-85 DEG C is warming up under rotating speed 400-800RPM, addition mass percent is 3-8% initiator solutions, constant temperature is pre-
Poly- 0.5-1.5h, you can obtain prepolymer；
（4）The aqueous effect pigment of amide modifications aligns the preparation of agent：Remaining pre-emulsion, pre-emulsion are added dropwise into prepolymer
1.5-4.0h at the uniform velocity completion of dropping, while remaining initiator solution, initiator solution 2.0-4.5h at the uniform velocity completion of dropping, drop is added dropwise
Plus during keep rotating speed to be 400-800RPM, temperature is 75-85 DEG C, keeping temperature 75-85 after all materials completion of dropping
DEG C insulation 0.5-2.0h, then 80-95 DEG C of insulation 0.5-3.0h is warming up to, it is subsequently cooled to 20-40 DEG C, acyl is made in filtering and discharging
Amine modified water-soluble effect pigment aligns agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109852216A (en) * | 2018-12-13 | 2019-06-07 | 清远市浩宇化工科技有限公司 | A kind of water-based metal metallic finishe |
| CN115141306A (en) * | 2022-08-11 | 2022-10-04 | 河南同胜新材料科技有限公司 | Polymethacrylimide foamed plastic and preparation method thereof |
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| CN103588929A (en) * | 2013-11-15 | 2014-02-19 | 马钢(集团)控股有限公司 | Pure acrylic emulsion, preparation method thereof and electrical steel paint |
| CN105399883A (en) * | 2015-12-31 | 2016-03-16 | 东莞市隆海新材料科技有限公司 | Directional arraying agent for waterborne effect pigment, and preparation method and application thereof |
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| CN102344710A (en) * | 2011-07-04 | 2012-02-08 | 何健 | Water-based lamellar pigment orientation arrangement agent and manufacturing method thereof |
| CN103588929A (en) * | 2013-11-15 | 2014-02-19 | 马钢(集团)控股有限公司 | Pure acrylic emulsion, preparation method thereof and electrical steel paint |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109852216A (en) * | 2018-12-13 | 2019-06-07 | 清远市浩宇化工科技有限公司 | A kind of water-based metal metallic finishe |
| CN109852216B (en) * | 2018-12-13 | 2021-04-30 | 清远市浩宇化工科技有限公司 | Water-based metal flashing paint |
| CN115141306A (en) * | 2022-08-11 | 2022-10-04 | 河南同胜新材料科技有限公司 | Polymethacrylimide foamed plastic and preparation method thereof |
| CN115141306B (en) * | 2022-08-11 | 2023-08-08 | 河南同胜新材料科技有限公司 | Polymethacrylimide foam plastic and preparation method thereof |
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| CN107151293B (en) | 2019-09-24 |
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