CN105802307A - Fluorescent modified nanometer SiO2/fluorine-containing polymer ultraviolet-curable coating and preparing method thereof - Google Patents
Fluorescent modified nanometer SiO2/fluorine-containing polymer ultraviolet-curable coating and preparing method thereof Download PDFInfo
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- CN105802307A CN105802307A CN201610271065.9A CN201610271065A CN105802307A CN 105802307 A CN105802307 A CN 105802307A CN 201610271065 A CN201610271065 A CN 201610271065A CN 105802307 A CN105802307 A CN 105802307A
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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
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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- C08F222/00—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 a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
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- C08F222/12—Esters of phenols or saturated alcohols
- C08F222/20—Esters containing oxygen in addition to the carboxy oxygen
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention discloses a fluorescent modified nanometer SiO2/fluorine-containing polymer ultraviolet-curable coating. The ultraviolet-curable coating is prepared from the following ingredients in percentage by weight: 15%-20% of fluorescent SiO2 nanometer particle, 40%-50% of fluorine-containing acrylic resin solution, 10%-15% of active diluted monomer, 10%-20% of xylene, 2%-7% of ultraviolet light initiating agent and 1%-5% of assisting agent. The invention further discloses a preparing method of the coating. The coating has super-hydrophobicity performance and self-cleaning performance, a contact angle between the coating and water exceeds 140 degrees, and fluorescence of the coating can provides a detecting method which is simple and easy to operate for using safety and using reliability of an electronic product.
Description
Technical field
The present invention relates to technical field of coatings, be specially a kind of fluorescence modified Nano SiO2/ fluoropolymer UV-curing
Change coating and preparation method thereof.
Background technology
After Bayer A.G successfully develops photocureable coating, UV-curing technology has obtained swift and violent development,
Ultraviolet-curing paint product is continuously increased, and quality is also stepping up.UV-curing technology have low energy consumption, high production capacity,
The advantages such as low stain, in today that environmental consciousness is surging, more show its importance.
Along with the development of coatings industry, occurring in that various functional coating on the market, fluorescent paint is exactly wherein one
Kind.At present, fluorescent paint on the market is many based on addition type coating, by adding fluorescent material to reach the effect of fluorescence.
In prior art, a lot of coating can not reach the performance of preferable fluorescent effect, even coating itself and be affected.It addition,
Although some fluorescent paints can reach certain fluorescent effect, but the performance of coating itself is the most unstable, there is easy to wear, suction
Attached binding dust and the problem such as durability degree is low.Therefore, develop a kind of preparation method that operation is simple, obtain a kind of new fluorescence and
The super-hydrophobicity wear-resistant paint of UV curable, thus expand its range of application, just seem particularly necessary.
Summary of the invention
Technical problem solved by the invention is to provide a kind of fluorescence modified Nano SiO2/ fluoropolymer UV-curing
Change coating and preparation method thereof, thus solve the problem in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A kind of fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, this ultraviolet-curing paint includes following weight
The component of amount percentage composition: fluorescence SiO2Nanoparticle 15%-20%, fluoroacrylic resin solution 40%-50%, activity dilution is single
Body 10%-15%, dimethylbenzene 10%-20%, ultraviolet initiator 2%-7%, auxiliary agent 1%-5%.
Described fluorescence nano SiO2Particle diameter is 40-90nm.
Described fluorescence SiO2Nanoparticle is adopted and is prepared with the following method: in single necked round bottom flask, adds a certain amount of different
Hydrogen thiocyanate fluorescein and appropriate DMF, add the 3-aminopropan of 2 times of Fluorescein isothiocyanate weight
Ethyl triethoxy silicane alkane, at N2Reaction 6 hs are stirred at room temperature under protection, and rotary evaporation removes the 3-aminopropyl triethoxy of excess
Silane, products therefrom (Si-FITC) pentane washs, and is vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add one
Quantitative hexamethylene and Triton X-100, be quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein under stirring
VHexamethylene:VTriton X-100:VAmmonia=15:4:2, then adds appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, in dark
Under the conditions of stirring reaction 12 h, product add excess diethyl ether, filter, filtering residue with apparatus,Soxhlet's purify, obtain fluorescence SiO2Nanometer
Granule.
Described fluoroacrylic resin solution manufacturing method is as follows: at 500 mL equipped with reflux condensing tube, thermometer, machinery
In the porous dry round-bottomed flask of agitator and ultrasonic probe, adding a certain amount of dimethylbenzene and butyl acetate solvent, machinery stirs
Mix down and be passed through N2To remove O2, open ultrasonic wave added, after question response temperature reaches 75 DEG C-85 DEG C, drip methacrylic acid ten difluoro
Heptyl ester, double trimethylolpropane acrylate and the mixed liquor of initiator, control to drip off at 3-4 h, insulation reaction 5-6 h.Cold
But to discharging after room temperature, fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate and double trihydroxy methyls third are obtained
The thing mass ratio of alkane acrylate is 1:2, and initiator is azodiisobutyronitrile.
Described activity diluting monomer is 2-(Acryloyloxy)ethanol, n-butyl acrylate, tripropylene glycol diacrylate, 2-benzene oxygen
One or more in base ethyl propylene acid esters.
Described ultraviolet initiator is in Irgacure184, Irgacure369, Irgacure1490, Darocur1173
One or more.
Described auxiliary agent includes polymerization inhibitor, defoamer, levelling agent.
The present invention also provides for this fluorescence modified Nano SiO2The preparation method of/fluoropolymer ultraviolet-curing paint, should
Method comprises the following steps: (1), in single necked round bottom flask, adds a certain amount of Fluorescein isothiocyanate and appropriate N, N-
Dimethylformamide, adds the APTES of 2 times of Fluorescein isothiocyanate weight, at N2Under protection
Reaction 6 hs are stirred at room temperature, and rotary evaporation removes the APTES of excess, and products therefrom (Si-FITC) is used
Pentane washs, and is vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add a certain amount of hexamethylene and Polyethylene Glycol is pungent
Base phenyl ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:4:
2, then add appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, stirring reaction 12 h under dark condition, product adds
Entering excess diethyl ether, filter, filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.(2), at 500 mL equipped with backflow
In the porous dry round-bottomed flask of condensing tube, thermometer, mechanical agitator and ultrasonic probe, add a certain amount of dimethylbenzene and second
Acid butyl ester solvent, is passed through N under mechanical agitation2To remove O2, open ultrasonic wave added, after question response temperature reaches 75 DEG C-85 DEG C, drip
Methylate dodecafluorhe-ptylacrylate, double trimethylolpropane acrylate and the mixed liquor of initiator, about 3-4 h drips off, and protects
Temperature reaction 5-6 h.It is cooled to discharging after room temperature, obtains fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate
Being 1:2 with the thing mass ratio of double trimethylolpropane acrylate, initiator is azodiisobutyronitrile.(3), by fluorescence SiO2Receive
Rice corpuscles 15%-20%, fluoroacrylic resin solution 40%-50%, activity diluting monomer 10%-15%, dimethylbenzene 10%-20% are purple
Outer light trigger 2%-7%, auxiliary agent 1%-5% phase mixes, and stirs, and forms mixture, obtains ultraviolet-curing paint.
The present invention has the advantage that relative to prior art and beneficial effect:
(1) Nano-meter SiO_2 with fluorescence phenomenon of the present invention2The ultraviolet-curing paint of/fluoropolymer modification has simultaneously
Super-hydrophobicity and self-cleaning performance, to the contact angle of water more than 140 °.
(2) fluorescence that this coating has can be that the safety and reliability that electronic product uses provides simple inspection
Survey means.
(3) the preparation method technical maturity of the present invention, step is simple, with low cost, is suitable for large-scale promotion, application prospect
Wide.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
A kind of fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, the weight of this ultraviolet cured paint composition
Amount percentage composition is: fluorescence SiO2Nanoparticle 16%, fluoroacrylic resin solution 45%, activity diluting monomer 13%, dimethylbenzene
17%, ultraviolet initiator 5% and auxiliary agent 4%.
The Nano-meter SiO_2 with fluorescence phenomenon of the present embodiment2The ultraviolet-curing paint preparation side that/fluoropolymer is modified
Method step is as follows: (1), in single necked round bottom flask, adds a certain amount of Fluorescein isothiocyanate and appropriate N, N-dimethyl
Methanamide, adds the APTES of 2 times of Fluorescein isothiocyanate weight, at N2The lower room temperature of protection is stirred
Mixing reaction 6 h, rotary evaporation removes the APTES of excess, and products therefrom (Si-FITC) is washed with pentane
Wash, and be vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add a certain amount of hexamethylene and Polyethylene Glycol octyl phenyl
Ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:4:2, then
Adding appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, stirring reaction 12 h under dark condition, product adds excess
Ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.(2), 500 mL equipped with reflux condensing tube,
In the porous dry round-bottomed flask of thermometer, mechanical agitator and ultrasonic probe, add a certain amount of dimethylbenzene and butyl acetate
Solvent, is passed through N under mechanical agitation2To remove O2, open ultrasonic wave added, after question response temperature reaches 75 DEG C, drip methacrylic acid
Ten difluoro heptyl esters, double trimethylolpropane acrylate and the mixed liquor of initiator, 3 h drip off, insulation reaction 5 h.It is cooled to
Discharging after room temperature, obtains fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate and double trimethylolpropane third
The thing mass ratio of olefin(e) acid ester is 1:2, and initiator is azodiisobutyronitrile.(3), weigh according to above-mentioned formula, be 40-by particle diameter
The fluorescence SiO of 90nm2Nanoparticle, fluoroacrylic resin solution, activity diluting monomer, dimethylbenzene, ultraviolet initiator and
Auxiliary agent stirs, and forms mixture, obtains ultraviolet-curing paint.
Wherein activity diluting monomer is 2-(Acryloyloxy)ethanol, and ultraviolet initiator is Irgacure184, and auxiliary agent uses inhibition
Agent, defoamer, levelling agent, the mixture of color filters.
Embodiment 2
A kind of fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, the weight of this ultraviolet cured paint composition
Amount percentage composition is: fluorescence SiO2Nanoparticle 18%, fluoroacrylic resin solution 48%, activity diluting monomer 12%, dimethylbenzene
14%, ultraviolet initiator 4% and auxiliary agent 4%.
The Nano-meter SiO_2 with fluorescence phenomenon of the present embodiment2The ultraviolet-curing paint preparation side that/fluoropolymer is modified
Method step is as follows: (1), in single necked round bottom flask, adds a certain amount of Fluorescein isothiocyanate and appropriate N, N-dimethyl
Methanamide, adds the APTES of 2 times of Fluorescein isothiocyanate weight, at N2The lower room temperature of protection is stirred
Mixing reaction 6 h, rotary evaporation removes the APTES of excess, and products therefrom (Si-FITC) is washed with pentane
Wash, and be vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add a certain amount of hexamethylene and Polyethylene Glycol octyl phenyl
Ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:4:2, then
Adding appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, stirring reaction 12 h under dark condition, product adds excess
Ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.(2), 500 mL equipped with reflux condensing tube,
In the porous dry round-bottomed flask of thermometer, mechanical agitator and ultrasonic probe, add a certain amount of dimethylbenzene and butyl acetate
Solvent, is passed through N under mechanical agitation2To remove O2, open ultrasonic wave added, after question response temperature reaches 85 DEG C, drip methacrylic acid
Ten difluoro heptyl esters, double trimethylolpropane acrylate and the mixed liquor of initiator, 4 h drip off, insulation reaction 6 h.Cooling
Discharging to room temperature, obtains fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate and double trimethylolpropane
The thing mass ratio of acrylate is 1:2, and initiator is azodiisobutyronitrile.(3), weigh according to above-mentioned formula, by fluorescence SiO2
Nanoparticle, fluoroacrylic resin solution, activity diluting monomer, dimethylbenzene, ultraviolet initiator and auxiliary agent stir, shape
Resulting mixture, obtains ultraviolet-curing paint.
Wherein activity diluting monomer is n-butyl acrylate, and ultraviolet initiator is Irgacure369, and auxiliary agent uses inhibition
Agent, defoamer, levelling agent, the mixture of color filters.
Embodiment 3
A kind of fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, the weight of this ultraviolet cured paint composition
Amount percentage composition is: fluorescence SiO2Nanoparticle 19%, fluoroacrylic resin solution 43%, activity diluting monomer 15%, dimethylbenzene
15%, ultraviolet initiator 3% and auxiliary agent 5%.
The Nano-meter SiO_2 with fluorescence phenomenon of the present embodiment2The ultraviolet-curing paint preparation side that/fluoropolymer is modified
Method step is as follows: (1), in single necked round bottom flask, adds a certain amount of Fluorescein isothiocyanate and appropriate N, N-dimethyl
Methanamide, adds the APTES of 2 times of Fluorescein isothiocyanate weight, at N2The lower room temperature of protection is stirred
Mixing reaction 6 h, rotary evaporation removes the APTES of excess, and products therefrom (Si-FITC) is washed with pentane
Wash, and be vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add a certain amount of hexamethylene and Polyethylene Glycol octyl phenyl
Ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:4:2, then
Adding appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, stirring reaction 12 h under dark condition, product adds excess
Ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.(2), 500 mL equipped with reflux condensing tube,
In the porous dry round-bottomed flask of thermometer, mechanical agitator and ultrasonic probe, add a certain amount of dimethylbenzene and butyl acetate
Solvent, is passed through N under mechanical agitation2To remove O2, open ultrasonic wave added, after question response temperature reaches 80 DEG C, drip methacrylic acid
Ten difluoro heptyl esters, double trimethylolpropane acrylate and the mixed liquor of initiator, 3.5h drips off, insulation reaction 5.5h.Cooling
Discharging to room temperature, obtains fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate and double trimethylolpropane
The thing mass ratio of acrylate is 1:2, and initiator is azodiisobutyronitrile.(3), weigh according to above-mentioned formula, by fluorescence SiO2
Nanoparticle, fluoroacrylic resin solution, activity diluting monomer, dimethylbenzene, ultraviolet initiator and auxiliary agent stir, shape
Resulting mixture, obtains ultraviolet-curing paint.
Wherein activity diluting monomer is tripropylene glycol diacrylate, and ultraviolet initiator is Irgacure1490, auxiliary agent
Use polymerization inhibitor, defoamer, levelling agent, the mixture of color filters.
Embodiment 4
A kind of fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, the weight of this ultraviolet cured paint composition
Amount percentage composition is: fluorescence SiO2Nanoparticle 15%, fluoroacrylic resin solution 46%, activity diluting monomer 14%, dimethylbenzene
18%, ultraviolet initiator 3% and auxiliary agent 4%.
The Nano-meter SiO_2 with fluorescence phenomenon of the present embodiment2The ultraviolet-curing paint preparation side that/fluoropolymer is modified
Method step is as follows: (1), in single necked round bottom flask, adds a certain amount of Fluorescein isothiocyanate and appropriate N, N-dimethyl
Methanamide, adds the APTES of 2 times of Fluorescein isothiocyanate weight, at N2The lower room temperature of protection is stirred
Mixing reaction 6 h, rotary evaporation removes the APTES of excess, and products therefrom (Si-FITC) is washed with pentane
Wash, and be vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add a certain amount of hexamethylene and Polyethylene Glycol octyl phenyl
Ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:4:2, then
Adding appropriate 1-hexanol, tetraethyl orthosilicate and Si-FITC, stirring reaction 12 h under dark condition, product adds excess
Ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.(2), 500 mL equipped with reflux condensing tube,
In the porous dry round-bottomed flask of thermometer, mechanical agitator and ultrasonic probe, add a certain amount of dimethylbenzene and butyl acetate
Solvent, is passed through N under mechanical agitation2To remove O2, open ultrasonic wave added, after question response temperature reaches 78 DEG C, drip methacrylic acid
Ten difluoro heptyl esters, double trimethylolpropane acrylate and the mixed liquor of initiator, 4 h drip off, insulation reaction 5 h.It is cooled to
Discharging after room temperature, obtains fluoroacrylic resin solution, wherein dodecafluoroheptyl methacrylate and double trimethylolpropane third
The thing mass ratio of olefin(e) acid ester is 1:2, and initiator is azodiisobutyronitrile.(3), weigh according to above-mentioned formula, by fluorescence SiO2Receive
Rice corpuscles, fluoroacrylic resin solution, activity diluting monomer, dimethylbenzene, ultraviolet initiator and auxiliary agent stir, and are formed
Mixture, obtains ultraviolet-curing paint.
Wherein activity diluting monomer is 2-phenoxyethyl acrylate, and ultraviolet initiator is Darocur1173, auxiliary agent
Use polymerization inhibitor, defoamer, levelling agent, the mixture of color filters.
Embodiment 5
Fluorescence modified Nano SiO to embodiment 1-42/ fluoropolymer ultraviolet-curing paint carries out performance test, test knot
Fruit is shown in Table 1.
The fluorescence modified Nano SiO of table 1 embodiment 1-42/ fluoropolymer ultraviolet-curing paint carries out performance test
Result
As shown in Table 1, the fluorescence modified Nano SiO of the present invention2The hydrophobic performance of/fluoropolymer ultraviolet-curing paint, resistance to
Mill property and fluorescent effect are relatively good, and preparation technology is the simplest, is suitable for large-scale promotion, has a extensive future.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (10)
1. a fluorescence modified Nano SiO2/ fluoropolymer ultraviolet-curing paint, it is characterised in that: described ultraviolet light polymerization
Coating includes the component of following weight percentage: fluorescence SiO2Nanoparticle 15%-20%, fluoroacrylic resin solution 40%-
50%, activity diluting monomer 10%-15%, dimethylbenzene 10%-20%, ultraviolet initiator 2%-7%, auxiliary agent 1%-5%.
A kind of fluorescence modified Nano SiO the most according to claim 12/ fluoropolymer ultraviolet-curing paint, its feature
It is: described fluorescence nano SiO2Particle diameter is 40-90nm.
A kind of fluorescence modified Nano SiO the most according to claim 22/ fluoropolymer ultraviolet-curing paint, its feature
It is: described fluorescence SiO2Nanoparticle is adopted and is prepared with the following method: in single necked round bottom flask, adds isothiocyanic acid glimmering
Light element and DMF, add the APTES of 2 times of Fluorescein isothiocyanate weight,
At N2Reaction 6 hs are stirred at room temperature under protection, and rotary evaporation removes the APTES of excess, products therefrom
Si-FITC, washs with pentane, and is vacuum dried at 60 DEG C；Separately take a single necked round bottom flask, add hexamethylene and Polyethylene Glycol
Octyl phenyl ether, is quickly added dropwise over the ammonia of 5 appropriate mol/L, wherein V under stirringHexamethylene:VTriton X-100:VAmmonia=15:
4:2, then adds 1-hexanol, tetraethyl orthosilicate and Si-FITC, and stirring reaction 12 h under dark condition, product added
Amount ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Nano-particle.
A kind of fluorescence modified Nano SiO the most according to claim 12/ fluoropolymer ultraviolet-curing paint, its feature
It is: described fluoroacrylic resin solution is adopted and prepared with the following method: at 500 mL equipped with reflux condensing tube, temperature
In the porous dry round-bottomed flask of meter, mechanical agitator and ultrasonic probe, add dimethylbenzene and butyl acetate solvent, mechanical agitation
Under be passed through N2To remove O2, open ultrasonic wave added, after question response temperature reaches 75 DEG C-85 DEG C, dropping methacrylic acid ten difluoro heptan
Ester, double trimethylolpropane acrylate and the mixed liquor of initiator, control to drip off at 3-4 h, insulation reaction 5-6 h；Cooling
Discharging to room temperature, obtains fluoroacrylic resin solution.
A kind of fluorescence modified Nano SiO the most according to claim 42/ fluoropolymer ultraviolet-curing paint, its feature
It is: the thing mass ratio of described dodecafluoroheptyl methacrylate and double trimethylolpropane acrylate is 1:2.
A kind of fluorescence modified Nano SiO the most according to claim 52/ fluoropolymer ultraviolet-curing paint, its feature
It is: described initiator is azodiisobutyronitrile.
A kind of fluorescence modified Nano SiO the most according to claim 12/ fluoropolymer ultraviolet-curing paint, its feature
It is: described activity diluting monomer is 2-(Acryloyloxy)ethanol, n-butyl acrylate, tripropylene glycol diacrylate, 2-phenoxy group
One or more in ethyl propylene acid esters.
A kind of fluorescence modified Nano SiO the most according to claim 12/ fluoropolymer ultraviolet-curing paint, its feature
It is: described ultraviolet initiator is in Irgacure184, Irgacure369, Irgacure1490, Darocur1173
Plant or several.
9. according to a kind of fluorescence modified Nano SiO described in any one of claim 1-82/ fluoropolymer ultraviolet light polymerization is coated with
Material, it is characterised in that: described auxiliary agent includes polymerization inhibitor, defoamer, levelling agent.
10. the method preparing ultraviolet-curing paint as claimed in claim 9, it is characterised in that: comprise the following steps:
(1), in single necked round bottom flask, add Fluorescein isothiocyanate and DMF, add 2 times of isothiocyanic acids
The APTES of fluorescein weight, at N2Reaction 6 hs are stirred at room temperature under protection, and rotary evaporation removes excess
APTES, products therefrom Si-FITC with pentane wash, and at 60 DEG C be vacuum dried；Separately take one
Single necked round bottom flask, adds hexamethylene and Triton X-100, is quickly added dropwise over 5 appropriate mol/L's under stirring
Ammonia, wherein VHexamethylene:VTriton X-100:VAmmonia=15:4:2, then adds 1-hexanol, tetraethyl orthosilicate and Si-FITC, in black
Stirring reaction 12 h under dark condition, product adds excess diethyl ether, filters, and filtering residue apparatus,Soxhlet's purifies, and obtains fluorescence SiO2Receive
Rice grain；(2), burn equipped with the porous dry round bottom of reflux condensing tube, thermometer, mechanical agitator and ultrasonic probe at 500 mL
In Ping, add and be passed through N under dimethylbenzene and butyl acetate solvent, mechanical agitation2To remove O2, open ultrasonic wave added, question response temperature
After reaching 75 DEG C-85 DEG C, dropping dodecafluoroheptyl methacrylate, double trimethylolpropane acrylate and the mixing of initiator
Liquid, 3-4 h drips off, insulation reaction 5-6 h；It is cooled to discharging after room temperature, obtains fluoroacrylic resin solution, wherein methyl
The thing mass ratio of dodecafluorhe-ptylacrylate and double trimethylolpropane acrylate is 1:2, and initiator is azodiisobutyronitrile；
(3), by the component of following percetage by weight: fluorescence SiO2Nanoparticle 15%-20%, fluoroacrylic resin solution 40%-50%,
Activity diluting monomer 10%-15%, dimethylbenzene 10%-20%, ultraviolet initiator 2%-7%, auxiliary agent 1%-5% phase mixes, and stirs,
Form mixture, obtain ultraviolet-curing paint.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977990A (en) * | 2017-04-06 | 2017-07-25 | 长沙理工大学 | A kind of antibacterial modification nano zine oxide/fluoropolymer ultraviolet-curing paint and preparation method thereof |
| CN113387352A (en) * | 2021-07-02 | 2021-09-14 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
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|---|---|---|---|---|
| CN102911540A (en) * | 2012-10-24 | 2013-02-06 | 华南理工大学 | Hydrophobic MMA (Methl Methacrylate) resin floor coating and preparation method thereof |
| CN103865372A (en) * | 2014-04-08 | 2014-06-18 | 中山职业技术学院 | Preparation method of fluorine-containing acrylic acid super-hydrophobic coating |
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2016
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911540A (en) * | 2012-10-24 | 2013-02-06 | 华南理工大学 | Hydrophobic MMA (Methl Methacrylate) resin floor coating and preparation method thereof |
| CN103865372A (en) * | 2014-04-08 | 2014-06-18 | 中山职业技术学院 | Preparation method of fluorine-containing acrylic acid super-hydrophobic coating |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106977990A (en) * | 2017-04-06 | 2017-07-25 | 长沙理工大学 | A kind of antibacterial modification nano zine oxide/fluoropolymer ultraviolet-curing paint and preparation method thereof |
| CN113387352A (en) * | 2021-07-02 | 2021-09-14 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
| CN113387352B (en) * | 2021-07-02 | 2022-07-12 | 西安交通大学 | Easily-dispersible modified graphene oxide and preparation method thereof |
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| CN105802307B (en) | 2018-04-03 |
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