CN106634185A - Halogen-free durable water-based polyurethane gravure fluorescence ink and preparation method thereof - Google Patents
Halogen-free durable water-based polyurethane gravure fluorescence ink and preparation method thereof Download PDFInfo
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- CN106634185A CN106634185A CN201611022119.4A CN201611022119A CN106634185A CN 106634185 A CN106634185 A CN 106634185A CN 201611022119 A CN201611022119 A CN 201611022119A CN 106634185 A CN106634185 A CN 106634185A
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
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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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/36—Hydroxylated esters of higher fatty acids
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a halogen-free durable water-based polyurethane gravure fluorescence ink which is prepared from the following raw materials in parts by weight: 4-5 parts of fine silicon dioxide aerogel, 1-2 parts of dodecyldimethyl betaine, 4-6 parts of tung oil, 17-20 parts of glycerol, 0.1-0.2 part of sodium methoxide, 6-8 parts of citric acid, 0.7-1 part of ethylenediamine, 50-60 parts of toluene diisocyanate, 60-70 parts of polyesterglycol, 0.8-2 parts of dibutyltin dilaurate, 1-2 parts of dimethylolpropionic acid, 2-3 parts of polyvinylpyrrolidone, 10-17 parts of water-based pigment, 3-4 parts of lauryl sodium sulfate, 1-2 parts of dimethyl silicone oil, 3-4 parts of sodium myristate soap, 2.4-3 parts of potassium fluotitanate, 1-2 parts of dihydrate gypsum powder, 0.8-1 part of bis imidazolidinyl urea, 0.1-0.3 part of ferrocenecarboxylic acid and 0.1-0.2 part of 96-98% sulfuric acid.
Description
Technical field
The present invention relates to technical field of ink, more particularly to a kind of Halogen durability aqueous polyurethane gravure fluorescent ink and
Its preparation method.
Background technology
Water color ink is the ink with water as solvent, and advantage of the water as solvent is：Nontoxic, free from extraneous odour, do not fire, and
The discharge capacity of VOC is greatly reduced, the pollution to environment is reduced, therefore has obtained development at full speed.And as water
A kind of water-based polyurethane ink in property ink, not only with water color ink safety and environmental protection the characteristics of, and have concurrently excellent resistance to
Mill property, the distinctive advantage of the polyurethane of resistance to water, chemical resistance and soft durometer adjustability, thus aqueous polyurethane is in ink
Application it is more and more extensive；But aqueous polyurethane is due to containing hydrophilic radical in molecular structure, thus with water-fast
Property congenital not enough weakness, the performance of aqueous polyurethane cannot match in excellence or beauty with traditional solvent borne polyurethane.Simultaneously with oil
The increasingly depleted of resource, people are sought for a kind of resource of natural reproducible to replace traditional non-renewable petroleum-type former
Expect to prepare Green Polymer Material；
Oleum Verniciae fordii is the distinctive natural reproducible resource of China, and its abundance, environmental protection contains three in Oleum Verniciae fordii molecular structure
Unsaturated conjugated double bond, during aqueous polyurethane strand can be introduced into, using during film-forming Oleum Verniciae fordii it is oxidation cross-linked
Reaction makes linear aqueous polyurethane form certain cross-linked structure, not only can so improve the resistance to water of aqueous polyurethane with
And combination property, while application of the biomass Renewable resource in polyurethane field can be improved, meet sending out for environmental protection
Exhibition is required；
Defect that resistance to water for aqueous polyurethane, solvent resistance aspect are present and comprehensive in order to further improve its
Can, many researcheres have all carried out fruitful initiative research work, and current research is concentrated mainly on modified to it
On.Cross-linking modified is to improve aqueous polyurethane water-resistance, solvent resistance, improve the most fruitful side such as mechanical property and hot property
Method.Based on this, the present invention utilizes the characteristic of the normal temperature oxidation self-crosslinking of Oleum Verniciae fordii base, by introducing Oleum Verniciae fordii base in polyurethane backbone
Tung oil-modified water-based polyurethane is prepared, and aqueous polyurethane printing-ink is prepared for as ink adhesive；
There is research to be prepared for high-quality fluorescent carbon quantum dot by microwave assisting method, and illustrate carbon quantum dot fluorescent ink and exist
Fluorescence character on skin and the fingerprint being imprinted on paper.The fluorescence quantum for being prepared is coated on paper, natural in air
It is dried, its fluorescent emission is remarkably reinforced (strengthen 40% by 14%).This phenomenon is with carbon quantum dot solution deposition in glass, gold
Due to caused fluorescent quenching phenomenon contrast of reuniting in category, silicon chip or plastic-substrates.Also, the paper of carbon quantum dot coating
Still there is excitation wavelength dependency, this shows, this carbon quantum dot solution can be used as a kind of new fluorescent ink.Different from it
His fluorescent ink, carbon quantum dot ink has fluorescence exciting wavelength dependency this distinguishing feature, can replace traditional ink, uses
In false proof and information recognize carbon quantum dot have it is nontoxic, inexpensive, prepare simple, good biocompatibility and be easy to function of surface
The advantages of change, particularly its superior fluorescence property and biocompatibility so as in necks such as bio-imaging, sensing and photoelectric devices
Domain has a wide range of applications.But in view of carbon quantum dot in the fluorescent quenching being dried or the easy generation of state of aggregation is stronger so as to
It is restricted in the application of solid state fluorescence equipment.In order to keep the physics and chemical stability of carbon quantum dot, prevent its acid or
Reunite under ionic condition, the application of carbon quantum dot is typically necessary and is further combined it with host material, in conventional research
In be mostly semiconductor-quantum-point and polymer is combined, but it is usually be connected using non-covalent bond with the macromole of labelling, knot
Structure is very unstable, in addition the environmental hazard of semiconductor-quantum-point itself, and the fluorescent polymer for making semiconductor-quantum-point labelling exists
The application in many fields such as biological medicine is restricted.As the green substitute of semiconductor-quantum-point, carbon quantum dot be polymerized
The compound of thing is arisen at the historic moment；
On the basis of the carbon quantum dot for preparing good fluorescence performance, itself and aqueous polyurethane are combined becomes a kind of new to the present invention
Type has the multi-functional pluralgel of fluorescence and temperature-responsive concurrently, while overcome carbon quantum dot in the easy fluorescent quenching of solid-state
Shortcoming.Additionally, prepare carbon-based hydrogel nano ink by the method, and by coating or intaglio printing, on different substrates
Print phosphor pattern.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of Halogen durability aqueous polyurethane gravure
Fluorescent ink and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of Halogen durability aqueous polyurethane gravure fluorescent ink, it is made up of the raw material of following weight parts：
Fine silicon dioxide aeroge 4-5, dodecyldimethylammonium hydroxide inner salt 1-2, Oleum Verniciae fordii 4-6, glycerol 17-20, Feldalat NM
0.1-0.2, citric acid 6-8, ethylenediamine 0.7-1, toluene di-isocyanate(TDI) 50-60, polyester diol 60-70, tin dilaurate two
Butyl tin 0.8-2, dihydromethyl propionic acid 1-2, polyvinylpyrrolidone 2-3, aqueous pigment 10-17, sodium lauryl sulphate 3-
4th, dimethicone 1-2, myristic acid soda soap 3-4, potassium fluotitanate 2.4-3, dihydrate gypsum powder 1-2, double imidazolidinyl urea 0.8-
1st, the sulphuric acid 0.1-0.2 of ferrocenecarboxylic acid 0.1-0.3,96-98%.
A kind of preparation method of described Halogen durability aqueous polyurethane gravure fluorescent ink, comprises the following steps：
（1）Above-mentioned dodecyldimethylammonium hydroxide inner salt is added in the deionized water of its weight 17-20 times, fluotitanic acid is added
Potassium, it is 60-70 DEG C to rise high-temperature, and insulated and stirred 8-10 minute, the hydrochloric acid of Deca 4-6mol/l, regulation pH is 2-3, and stirring mixes
20-30 minutes, obtain acid dispersion；
（2）Above-mentioned double imidazolidinyl urea is added in glycerol, is stirred, 4-10 minutes are preheated at 50-60 DEG C, added
Above-mentioned Oleum Verniciae fordii, Feldalat NM, in being sent to reactor, are passed through nitrogen, the stirring reaction 4-5 hour at 200-210 DEG C, discharging, plus
Enter the saturated sodium-chloride water solution of reacting rear material weight 1.8-2 times, stratification takes upper strata oil solution, obtains tung oil-modified two
First alcohol；
（3）Above-mentioned myristic acid soda soap is added in the dehydrated alcohol of its weight 10-13 times, it is 70-75 DEG C to rise high-temperature, plus
Enter ferrocenecarboxylic acid, insulated and stirred 10-16 minute, the sulphuric acid of Deca above-mentioned 96-98%, must be premixed stirring reaction 30-40 minute
Material；
（4）Above-mentioned citric acid, ethylenediamine are mixed, in being added to compound weight 38-40 times deionized water, polytetrafluoroethyl-ne is sent into
In alkene reaction kettle, 5-6 hours are incubated at 180-190 DEG C, cooling, takes supernatant at 10000-12000 rev/min of centrifugation 27-30 minute
Liquid, obtains carbon quantum dot solution；
（5）Above-mentioned fine silicon dioxide aeroge is added in the deionized water of its weight 20-30 times, ultrasonic 1-2 minutes, plus
Enter acid dispersion, stir, obtain colloidal silica dispersion；
（6）Above-mentioned polyvinylpyrrolidone is added in the deionized water of its weight 200-300 times, it is molten with above-mentioned carbon quantum dot
Liquid mixes, and ultrasonic 2-3 minutes, obtains carbon quantum dot dispersion liquid；
（7）Above-mentioned polyester diol is dried into 10-11 hours in 100-105 DEG C of vacuum drying oven, discharging cooling is sent into anti-
In answering kettle, nitrogen is passed through, it is 40-50 DEG C to adjust temperature of reaction kettle, and Deca toluene di-isocyanate(TDI) is incubated 20- after completion of dropping
30 minutes, above-mentioned premix material, dibutyl tin laurate are added, it is 60-70 DEG C to rise high-temperature, insulation reaction 100-120 minute,
Add above-mentioned dihydromethyl propionic acid, insulated and stirred 100-110 minute, add tung oil-modified dihydroxylic alcohols, stirring reaction 1-2 hour,
It is cooled to room temperature, adds above-mentioned carbon quantum dot dispersion liquid, colloidal silica dispersion, 2000-2300 rev/min of emulsification pretreatment 20-30 minute,
Obtain modified emulsion；
（8）Above-mentioned modified emulsion is mixed with remaining each raw material, grinding is uniform, obtains final product.
It is an advantage of the invention that：The present invention adopts tung oil-modified dihydroxylic alcohols as the raw material of synthesis of polyurethane so that Oleum Verniciae fordii
Contain conjugated double bond in modified polyurethane system, autoxidation crosslinking occurs during film-forming so that linear
Crosslinking or partial cross-linked structure are formed in aqueous polyurethane molecular structure, so as to substantially increase the resistance to water of aqueous polyurethane；
Simultaneously crosslinking points are defined in molecular chain structure through modified aqueous polyurethane, become three-dimensional net structure, improved
Its thermostability, the present invention on carbon quantum dot surface introduces amino by changing carbon matrix precursor-citric acid and ethylenediamine, fills out
Mend the defect on carbon quantum dot surface or make its surface produce energy potential well, make fluorescent emission more stable, so as to improve fluorescence quantum yield,
The fluorescence property for making carbon quantum dot is greatly improved, the present invention water color ink can by coating, gravure application black paper,
Different phosphor patterns printings are prepared on piezoid, Kapton, pet film substrate different
Phosphor pattern
Preferably, adhesive force is larger, Halogen good endurance for the ink smoothness of the present invention, and integrated quality is high.
Specific embodiment
A kind of Halogen durability aqueous polyurethane gravure fluorescent ink, it is made up of the raw material of following weight parts：
Fine silicon dioxide aeroge 4, dodecyldimethylammonium hydroxide inner salt 1, Oleum Verniciae fordii 4, glycerol 17, Feldalat NM 0.1, citric acid
6th, ethylenediamine 0.7, toluene di-isocyanate(TDI) 50, polyester diol 60, dibutyl tin laurate 0.8, dihydromethyl propionic acid 1,
Polyvinylpyrrolidone 2, aqueous pigment 10, sodium lauryl sulphate 3, dimethicone 1, myristic acid soda soap 3, potassium fluotitanate
2.4th, dihydrate gypsum powder 1, double imidazolidinyl urea 0.8, the sulphuric acid 0.1 of ferrocenecarboxylic acid 0.1,96%.
A kind of preparation method of described Halogen durability aqueous polyurethane gravure fluorescent ink, comprises the following steps：
（1）Above-mentioned dodecyldimethylammonium hydroxide inner salt is added in the deionized water of 17 times of its weight, potassium fluotitanate is added, is risen
High-temperature is 60 DEG C, insulated and stirred 8 minutes, the hydrochloric acid of Deca 4mol/l, and it is 2 to adjust pH, and stirring mixing 20 minutes obtains acid point
Dispersion liquid；
（2）Above-mentioned double imidazolidinyl urea is added in glycerol, is stirred, preheated 4 minutes at 50 DEG C, add above-mentioned paulownia
Oil, Feldalat NM, in being sent to reactor, are passed through nitrogen, stirring reaction 4 hours at 200 DEG C, discharging, add reacting rear material
The saturated sodium-chloride water solution that 1.8 times of weight, stratification takes upper strata oil solution, obtains tung oil-modified dihydroxylic alcohols；
（3）Above-mentioned myristic acid soda soap is added in the dehydrated alcohol of 10 times of its weight, it is 70 DEG C to rise high-temperature, and addition two is luxuriant
Iron formate, insulated and stirred 10 minutes, the sulphuric acid of Deca above-mentioned 96%, stirring reaction 30 minutes obtains premix material；
（4）Above-mentioned citric acid, ethylenediamine are mixed, in being added to 38 times of deionized waters of compound weight, politef is sent into
In reactor, 5 hours are incubated at 180 DEG C, cooling, 10000 revs/min are centrifuged 27 minutes, take supernatant, obtain carbon quantum dot molten
Liquid；
（5）Above-mentioned fine silicon dioxide aeroge is added in the deionized water of 20 times of its weight, ultrasound 1 minute adds acid
Property dispersion liquid, stirs, and obtains colloidal silica dispersion；
（6）Above-mentioned polyvinylpyrrolidone is added in the deionized water of 200 times of its weight, it is mixed with above-mentioned carbon quantum dot solution
Close, ultrasound 2 minutes obtains carbon quantum dot dispersion liquid；
（7）Above-mentioned polyester diol is dried 10 hours in 100 DEG C of vacuum drying oven, discharging cooling, in sending into reactor,
Nitrogen is passed through, it is 40 DEG C to adjust temperature of reaction kettle, and Deca toluene di-isocyanate(TDI) is incubated 20 minutes, in addition after completion of dropping
Premix material, dibutyl tin laurate are stated, it is 60 DEG C to rise high-temperature, and insulation reaction 100 minutes adds above-mentioned dihydroxymethyl third
Acid, insulated and stirred 100 minutes adds tung oil-modified dihydroxylic alcohols, stirring reaction 1 hour to be cooled to room temperature, add above-mentioned carbon quantum
Point dispersion liquid, colloidal silica dispersion, 2000 revs/min of emulsification pretreatments 20 minutes obtain modified emulsion；
（8）Above-mentioned modified emulsion is mixed with remaining each raw material, grinding is uniform, obtains final product.
The water color ink specimen page of the present invention is have printed using gravure printing adaptive instrument, water color ink does not have in printing process
Occur flying ink, the phenomenon of spanishing, ink is shifted well on ink roller, specimen page site is clear after print, mass colour is distinct；
Performance test：
Adhesive force：>=1 grade；
Glossiness：88°；
First dryness：14.7mm/30s；
Resistance to water：It is qualified.
Claims (2)
1. a kind of Halogen durability aqueous polyurethane gravure fluorescent ink, it is characterised in that it is by the raw material of following weight parts
Composition：
Fine silicon dioxide aeroge 4-5, dodecyldimethylammonium hydroxide inner salt 1-2, Oleum Verniciae fordii 4-6, glycerol 17-20, Feldalat NM
0.1-0.2, citric acid 6-8, ethylenediamine 0.7-1, toluene di-isocyanate(TDI) 50-60, polyester diol 60-70, tin dilaurate two
Butyl tin 0.8-2, dihydromethyl propionic acid 1-2, polyvinylpyrrolidone 2-3, aqueous pigment 10-17, sodium lauryl sulphate 3-
4th, dimethicone 1-2, myristic acid soda soap 3-4, potassium fluotitanate 2.4-3, dihydrate gypsum powder 1-2, double imidazolidinyl urea 0.8-
1st, the sulphuric acid 0.1-0.2 of ferrocenecarboxylic acid 0.1-0.3,96-98%.
2. a kind of preparation method of Halogen durability aqueous polyurethane gravure fluorescent ink as claimed in claim 1, its feature
It is to comprise the following steps：
（1）Above-mentioned dodecyldimethylammonium hydroxide inner salt is added in the deionized water of its weight 17-20 times, fluotitanic acid is added
Potassium, it is 60-70 DEG C to rise high-temperature, and insulated and stirred 8-10 minute, the hydrochloric acid of Deca 4-6mol/l, regulation pH is 2-3, and stirring mixes
20-30 minutes, obtain acid dispersion；
（2）Above-mentioned double imidazolidinyl urea is added in glycerol, is stirred, 4-10 minutes are preheated at 50-60 DEG C, added
Above-mentioned Oleum Verniciae fordii, Feldalat NM, in being sent to reactor, are passed through nitrogen, the stirring reaction 4-5 hour at 200-210 DEG C, discharging, plus
Enter the saturated sodium-chloride water solution of reacting rear material weight 1.8-2 times, stratification takes upper strata oil solution, obtains tung oil-modified two
First alcohol；
（3）Above-mentioned myristic acid soda soap is added in the dehydrated alcohol of its weight 10-13 times, it is 70-75 DEG C to rise high-temperature, plus
Enter ferrocenecarboxylic acid, insulated and stirred 10-16 minute, the sulphuric acid of Deca above-mentioned 96-98%, must be premixed stirring reaction 30-40 minute
Material；
（4）Above-mentioned citric acid, ethylenediamine are mixed, in being added to compound weight 38-40 times deionized water, polytetrafluoroethyl-ne is sent into
In alkene reaction kettle, 5-6 hours are incubated at 180-190 DEG C, cooling, takes supernatant at 10000-12000 rev/min of centrifugation 27-30 minute
Liquid, obtains carbon quantum dot solution；
（5）Above-mentioned fine silicon dioxide aeroge is added in the deionized water of its weight 20-30 times, ultrasonic 1-2 minutes, plus
Enter acid dispersion, stir, obtain colloidal silica dispersion；
（6）Above-mentioned polyvinylpyrrolidone is added in the deionized water of its weight 200-300 times, it is molten with above-mentioned carbon quantum dot
Liquid mixes, and ultrasonic 2-3 minutes, obtains carbon quantum dot dispersion liquid；
（7）Above-mentioned polyester diol is dried into 10-11 hours in 100-105 DEG C of vacuum drying oven, discharging cooling is sent into anti-
In answering kettle, nitrogen is passed through, it is 40-50 DEG C to adjust temperature of reaction kettle, and Deca toluene di-isocyanate(TDI) is incubated 20- after completion of dropping
30 minutes, above-mentioned premix material, dibutyl tin laurate are added, it is 60-70 DEG C to rise high-temperature, insulation reaction 100-120 minute,
Add above-mentioned dihydromethyl propionic acid, insulated and stirred 100-110 minute, add tung oil-modified dihydroxylic alcohols, stirring reaction 1-2 hour,
It is cooled to room temperature, adds above-mentioned carbon quantum dot dispersion liquid, colloidal silica dispersion, 2000-2300 rev/min of emulsification pretreatment 20-30 minute,
Obtain modified emulsion；
（8）Above-mentioned modified emulsion is mixed with remaining each raw material, grinding is uniform, obtains final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611022119.4A CN106634185A (en) | 2016-11-21 | 2016-11-21 | Halogen-free durable water-based polyurethane gravure fluorescence ink and preparation method thereof |
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| CN201611022119.4A CN106634185A (en) | 2016-11-21 | 2016-11-21 | Halogen-free durable water-based polyurethane gravure fluorescence ink and preparation method thereof |
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| CN201611022119.4A Pending CN106634185A (en) | 2016-11-21 | 2016-11-21 | Halogen-free durable water-based polyurethane gravure fluorescence ink and preparation method thereof |
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Cited By (2)
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| CN114317065A (en) * | 2021-12-24 | 2022-04-12 | 东莞理工学院 | Ferrocene group-based viscosity-controllable fluorosilicone oil and production method thereof |
| CN118206920A (en) * | 2024-05-16 | 2024-06-18 | 上海高邦印刷材料有限公司 | Water-based UV gloss oil capable of being used for rapidly detecting trace migration of photoinitiator |
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| CN103881049A (en) * | 2014-04-04 | 2014-06-25 | 中南林业科技大学 | Preparation method of eleostearic acid monoglyceride modified waterborne polyurethane emulsion |
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