CN107312117A - A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof - Google Patents
A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof Download PDFInfo
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- CN107312117A CN107312117A CN201710641085.5A CN201710641085A CN107312117A CN 107312117 A CN107312117 A CN 107312117A CN 201710641085 A CN201710641085 A CN 201710641085A CN 107312117 A CN107312117 A CN 107312117A
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- color paste
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- dispersible pigment
- pigment color
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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
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/22—Luminous paints
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
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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
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/14—Macromolecular compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Textile Engineering (AREA)
- Paints Or Removers (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof.It is related to dispersible pigment color paste, more particularly to a kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof.The covering power and fluorescent reflection intensity of the fluorescent emulsion of existing emulsion polymerization technique production can be improved.Include Protection glue, surfactant, emulsifying agent, dyestuff, deionized water, styrene, propylene cyanoacrylate class monomer, azodiisobutyronitrile, 5%HCl and 10%NaOH compounding.The present invention uses conventional emulsion polymerization technique, with faster polymerization speed.Then, the pH value of adjustment emulsion is to highly acid, and finally adjust pH value makes the particulate after flocculation be in stable state for alkalescence, so as to obtain the fluorescent pigment latex of big particle diameter.
Description
Technical field
The present invention relates to dispersible pigment color paste, more particularly to a kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof.
Background technology
Organic fluorescent pigment is also pigment with day-light fluorescence, and it absorbs visible ray and ultraviolet, ultraviolet light can be changed into one
The visible ray for determining color is reflected, and its total intensity of reflected light is much higher than general pigment, with very gorgeous color.It is glimmering
Delustering pigment is generally made up of fluorescent dye, vector resin, and vector resin provides certain physical and chemical performance, fluorescent dye dissolving
In vector resin.
When fluorescent pigment is applied to textile printing and dyeing or coating, it is necessary to pigment is previously prepared into aqueous color paste, generally make
Method has following three kinds：
First, block resin attrition grinding method, synthesizes block fluorescent pigment, is then comminuted into the micro- of 2~3 μm of particle diameter first
Grain, then adds dispersant, emulsifying agent, water and other auxiliary agent grinding distributions and obtains fluorescent pigment latex.The method is usually used
Para toluene sulfonamide-carbamide polymer resin, containing more free formaldehyde, while the phenomenons such as sedimentation are easily produced,
The emulsion particle diameter that the method is obtained is 2~3 μm, containing more coarse granule, easily causes mesh, the blocking or generation of roller version
The phenomenons such as spot.
2nd, emulsification-solidification method prepares aqueous fluorescent dispersible pigment color paste, first synthetic resin, is emulsified while dyeing, breast
Resolidification after the completion of change, obtains aqueous fluorescent dispersible pigment color paste.Use at present for benzoguanamine-carbamide tree
Fat, containing more free formaldehyde, while its particle diameter is 2~3 μm, containing larger coarse granule, also easily causes mesh, roller
The blocking of version produces the phenomenons such as spot.
3rd, emulsion polymerization prepares aqueous fluorescent dispersible pigment color paste, aqueous fluorescent dispersible pigment color paste prepared by emulsion polymerization, tool
There is particle diameter small, mesh, the blocking of roller version are not easily caused or the phenomenons such as spot are produced, simultaneously because using styrene, methyl-prop
E pioic acid methyl ester, propylene cyanogen, GMA, hydroxy propyl methacrylate, ethyl acrylate and vinylacetate
Deng monomer synthesis, formaldehyde is not contained, the problem of 2 kinds of methods of the above are produced thoroughly is solved.But emulsion polymerization typically results in breast
The particle diameter of liquid is 100~200nm, and the wavelength of visible ray is 380~780nm, and the particle diameter of latex particle is less than visible wavelength
Half when, be easily caused light penetration fluorescent pigment, produce the reflected light not low problem of the dark weak, covering power of strong, fluorescence.
Application for a patent for invention (CN 101787100 B, Yi Zhongshui disclosed in State Intellectual Property Office 2011.08.17
The synthesis technique of newborn type fluorescent pigment) a kind of synthesis technique of water-emulsion fluorescent pigment is disclosed, mainly including emulsification process, kind
Sub- emulsion synthesis procedure, dropwise reaction process and postprocessing working procedures；The present invention is to prepare emulsion by emulsification process first；Again
The 5%-20% that the emulsion of preparation takes its total amount is synthesized into seed emulsion, dropwise reaction process and post processing work are then carried out again
Sequence.
Application for a patent for invention (CN 105482019 A, Yi Zhongnai disclosed in State Intellectual Property Office 2016.04.13
Formaldehydeless fluorescent pigment latex of high temperature and preparation method thereof) a kind of fluorescent pigment latex and preparation method thereof is disclosed, it is described glimmering
Delustering pigment emulsion includes following weight component：Polymerized monomer 100%, emulsifying agent 0.5%~10%, initiator 0.01%~
10%, colouring agent 0.001%~20%, deionized water 50%~500%.
Emulsion polymerization is described above and prepares aqueous fluorescent dispersible pigment color paste, but does not all refer to the control of emulsion particle diameter
System, and the control of emulsion particle diameter have impact on the covering power of mill base, so as to have influence on the performance of stamp or application product.Using thin breast
Liquid polymerization technique, equally can obtain the emulsion of greater particle size, but polymerization speed is extremely slow, while polymer concentration is relatively low,
The need for industrial production can not being met.
The content of the invention
There is provided a kind of screening for the fluorescent emulsion that can improve existing emulsion polymerization technique production for problem above by the present invention
Aqueous fluorescent dispersible pigment color paste of lid power and fluorescent reflection intensity and preparation method thereof.
The technical scheme is that：Include the component of following parts by weight:
The Protection glue is hydroxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, one kind of PVP
Or several mixtures.
The surfactant is sodium laurate.
The emulsifying agent is the mixture of anion emulsifier and nonionic emulsifier, and the anion emulsifier is carbon containing
12~16 carboxylic acid sodium salt, its mass percent is 20%~40%；The nonionic emulsifier be 13 carbon APEOs,
One or more of mixtures of 15 carbon APEOs and 18 carbon APEOs, its mass percent be 60%~
80%.
A kind of preparation method of aqueous fluorescent dispersible pigment color paste, comprises the following steps：
S1, Protection glue, emulsifying agent and basic-dyeable fibre be added in deionized water, aqueous phase liquid is made in stirring and dissolving；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in there-necked flask add 5%-10% emulsion, be warming up to 80 ± 2 DEG C, remaining emulsion, 2- be slowly added dropwise
Completion of dropping in 3h, drips off insulation 2-3h；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2~2.5, then be incubated 1-2h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjustment pH value to 7.5~8.5 are incubated 1-2h, filtering
Discharging, obtains big particle diameter aqueous fluorescent dispersible pigment color paste.
The present invention synthesizes the conventional emulsions that particle diameter is 100~200nm at work, first, can be poly- using conventional emulsions
Technique is closed, with faster polymerization speed.Then, the pH value of adjustment emulsion is to highly acid, now emulsifying agent anion emulsifier
Lose protecting effect, emulsion particle loss of stability and produce flocculation, due to having nonionic emulsifier and nonionic Protection glue
In the presence of particle diameter, which is risen to after 450~550nm, reaches stabilization, and finally adjust pH value makes the particulate after flocculation in stable for alkalescence
State, so as to obtain the fluorescent pigment latex of big particle diameter.
Embodiment
The present invention includes the component of following parts by weight:
The Protection glue is hydroxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, one kind of PVP
Or several mixtures.
The surfactant is sodium laurate.
The emulsifying agent is the mixture of anion emulsifier and nonionic emulsifier, and the anion emulsifier is carbon containing
12~16 carboxylic acid sodium salt, its mass percent is 20%~40%；The nonionic emulsifier be 13 carbon APEOs,
One or more of mixtures of 15 carbon APEOs and 18 carbon APEOs, its mass percent be 60%~
80%.
A kind of preparation method of aqueous fluorescent dispersible pigment color paste, comprises the following steps：
S1, Protection glue, emulsifying agent and basic-dyeable fibre be added in deionized water by corresponding parts by weight, stirring and dissolving,
Aqueous phase liquid is made；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in agitator, the there-necked flask of condenser add 5%-10% emulsion, be warming up to 80 ± 2 DEG C, delay
It is slow that completion of dropping in remaining emulsion, 2-3h is added dropwise, drip off insulation 2-3h；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2~2.5, then be incubated 1-2h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjustment pH value to 7.5~8.5 are incubated 1-2h, filtering
Discharging, obtains big particle diameter aqueous fluorescent dispersible pigment color paste.Particle diameter is big when coating film forming is dried, after moisture is separated out, and mill base distribution is equal
It is even, the degree of accuracy of color matching will not be improved with moisture to surface migration.
Acrylic ester monomer can be methyl methacrylate, ethyl acrylate, hydroxy propyl methacrylate or methyl-prop
Olefin(e) acid ethylene oxidic ester.
The invention will be further described with comparative example with reference to embodiments, but is not limited to this.
Embodiment and comparative example are raw materials used unless otherwise indicated, are technical grade commercially available product.
Embodiment one
The present invention includes following components by weight percent
Protection glue, emulsifying agent and basic-dyeable fibre S1, are added in deionized water by it at work, and stirring and dissolving is made
Aqueous phase liquid；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in agitator, the there-necked flask of condenser add 5% emulsion, be warming up to 80 DEG C, be slowly added dropwise surplus
Completion of dropping in remaining emulsion, 2h, drips off insulation 2h；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2, then be incubated 1h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjust pH value to 7.5, are incubated 2h, filtering and discharging is obtained
To big particle diameter aqueous fluorescent dispersible pigment color paste.
Embodiment two
The present invention includes following components by weight percent
Protection glue, emulsifying agent and basic-dyeable fibre S1, by corresponding parts by weight are added to deionized water by it at work
In, aqueous phase liquid is made in stirring and dissolving；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in agitator, the there-necked flask of condenser add 5%-10% emulsion, be warming up to 81 DEG C, slowly
Completion of dropping in remaining emulsion, 2h is added dropwise, insulation 3h is dripped off；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2.5, then be incubated 2h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjust pH value to 8.5, are incubated 2h, filtering and discharging is obtained
To big particle diameter aqueous fluorescent dispersible pigment color paste.
Embodiment three
The present invention includes following components by weight percent
S1, Protection glue, emulsifying agent and basic-dyeable fibre be added in deionized water by corresponding parts by weight, stirring and dissolving,
Aqueous phase liquid is made；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in agitator, the there-necked flask of condenser add 5%-10% emulsion, be warming up to 82 DEG C, slowly
Completion of dropping in remaining emulsion, 3h is added dropwise, insulation 2.5h is dripped off；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2.5, then be incubated 2h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjust pH value to 8.5, are incubated 1h, filtering and discharging is obtained
To big particle diameter aqueous fluorescent dispersible pigment color paste.
For embodiment one, embodiment two and embodiment three, emulsion particle diameter is tested respectively and the test of black and white lattice method is covered
Power, data are as follows
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Surface area average grain diameter nm | 473 | 514 | 489 |
| Covering power g/m2 | 78 | 73 | 75 |
As can be seen from the above table, particle diameter produced by the present invention and covering power are significantly greater than aqueous fluorescent face of the prior art
Expect mill base.
Claims (5)
1. a kind of aqueous fluorescent dispersible pigment color paste, it is characterised in that include the component of following parts by weight:
2. a kind of aqueous fluorescent dispersible pigment color paste according to claim 1, it is characterised in that the Protection glue is that methylol is fine
Tie up element, hydroxypropyl cellulose, polyvinyl alcohol, one or more of mixtures of PVP.
3. a kind of aqueous fluorescent dispersible pigment color paste according to claim 1, it is characterised in that the surfactant is bay
Sour sodium.
4. a kind of aqueous fluorescent dispersible pigment color paste according to claim 1, it is characterised in that the emulsifying agent is anion breast
The mixture of agent and nonionic emulsifier, the anion emulsifier is carbon containing 12~16 carboxylic acid sodium salt, its quality percentage
Number is 20%~40%；The nonionic emulsifier is 13 carbon APEOs, 15 carbon APEOs and 18 carbon polies
One or more of mixtures of oxygen vinethene, its mass percent is 60%~80%.
5. the preparation method of the aqueous fluorescent dispersible pigment color paste described in a kind of claim 1, it is characterised in that comprise the following steps：
S1, Protection glue, emulsifying agent and basic-dyeable fibre be added in deionized water, aqueous phase liquid is made in stirring and dissolving；
S2, by styrene, acrylic ester monomer and propylene cyanogen mixed dissolution in azodiisobutyronitrile；
S3, S2 resulting solutions are slowly added into aqueous phase liquid made from S1, emulsion is obtained after high-shear emulsifying；
S4, in there-necked flask add 5%-10% emulsion, be warming up to 80 ± 2 DEG C, be slowly added dropwise in remaining emulsion, 2-3h
Completion of dropping, drips off insulation 2-3h；
S5, the HCl solution that mass fraction is 5% is slowly added dropwise again adjusts pH value to 2~2.5, then be incubated 1-2h；
S6, last, the NaOH solution that dropwise addition mass fraction is 10%, adjustment pH value to 7.5~8.5, insulation 1-2h are filtered out
Material, obtains big particle diameter aqueous fluorescent dispersible pigment color paste.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710641085.5A CN107312117A (en) | 2017-07-31 | 2017-07-31 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710641085.5A CN107312117A (en) | 2017-07-31 | 2017-07-31 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535850A (en) * | 2018-12-04 | 2019-03-29 | 扬州辰鑫新材料科技有限公司 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof |
| CN109535861A (en) * | 2018-12-04 | 2019-03-29 | 扬州辰鑫新材料科技有限公司 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof using solvent dye preparation |
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| CN103555069A (en) * | 2013-10-21 | 2014-02-05 | 扬州大学 | Preparation method of aqueous daylight fluorescent pigment color paste |
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| CN106133051A (en) * | 2014-01-30 | 2016-11-16 | 巴斯夫欧洲公司 | The resin carrier emulsion polymerization of hydrophobic monomer |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535850A (en) * | 2018-12-04 | 2019-03-29 | 扬州辰鑫新材料科技有限公司 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof |
| CN109535861A (en) * | 2018-12-04 | 2019-03-29 | 扬州辰鑫新材料科技有限公司 | A kind of aqueous fluorescent dispersible pigment color paste and preparation method thereof using solvent dye preparation |
| CN109535861B (en) * | 2018-12-04 | 2021-01-01 | 扬州辰鑫新材料科技有限公司 | Preparation method of water-based fluorescent pigment color paste prepared from solvent dye |
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