CN104479437A - Preparation method for super-hydrophobic self-luminous coating - Google Patents

Preparation method for super-hydrophobic self-luminous coating Download PDF

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CN104479437A
CN104479437A CN201510004648.0A CN201510004648A CN104479437A CN 104479437 A CN104479437 A CN 104479437A CN 201510004648 A CN201510004648 A CN 201510004648A CN 104479437 A CN104479437 A CN 104479437A
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super
coating
preparation
luminous
hydrophobic self
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CN104479437B (en
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石小迪
鲁希华
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Donghua University
National Dong Hwa University
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Donghua University
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Abstract

The invention provides a preparation method for a super-hydrophobic self-luminous coating. The method comprises the following two steps of 1, uniformly mixing a high-molecular polymer monomer, a cross-linking agent, an initiating agent, nano-particles and long-lasting phosphor materials to obtained a mixture; 2, uniformly coating the surface of a base material with the mixture, and carrying out polymerization to obtain the super-hydrophobic self-luminous coating. The preparation method for the super-hydrophobic self-luminous coating overcomes the shortcomings of the prior art, the application range of the long-lasting phosphor materials is widened, and meanwhile the problem that the super-hydrophobic self-luminous coating is decomposed or the luminous intensity is reduced when water is encountered is solved. The preparation method for the super-hydrophobic self-luminous coating is simple in process and high in universality, and the manufacturing cost is saved.

Description

A kind of preparation method of super-hydrophobic self-luminous coating
Technical field
The present invention relates to a kind of by carrying out coated and doping to long after glow luminous material, prepare the method for super-hydrophobic self-luminous coating, belong to coating technology field.
Background technology
Long after glow luminous material is a kind of " green " source material, namely under natural light or artificial light irradiate, store optical radiation energy, after light source cuts off, still can discharge the energy of storage with the form of visible ray, presenting the bright light that can distinguish, is desirable emergent instruction light source.Along with going deep into of Recent study, its time of persistence has also brought up to tens hours from a few second.There is illumination functions, the effect of emergent instruction can be played, but the long after glow luminous material of a lot of good luminescence property is very responsive to water, easily decomposes, luminescent decay, finally lose luminous power in damp atmosphere.Therefore how making long after glow luminous material avoid the interference of steam, and can be used for the fields such as moist or under harsh environmental conditions emergency lighting or instruction, for further expanding its range of application, there is very important Research Significance.
Superhydrophobic surface material refers to that water droplet is rounded at material surface, and its contact angle is greater than 150 degree, therefore shows automatically cleaning, a series of excellent properties such as anti-pollution.By manufacturing suitable surfaceness or the modification by low-surface energy substance at material surface, super-hydrophobic surface can be prepared.Such material all has broad application prospects in national defence, industry, agricultural, medical science and daily life.
At present, the fabrication & properties research of the super-hydrophobic self-luminous coating related in the present invention there is not yet bibliographical information.
Summary of the invention
The technical problem to be solved in the present invention is the interference how making long after glow luminous material avoid steam, and can be used for moist or under harsh environmental conditions emergency lighting or instruction.
In order to solve the problems of the technologies described above, technical scheme of the present invention is to provide a kind of preparation method of super-hydrophobic self-luminous coating, it is characterized in that: the method is made up of following 2 steps:
Step 1: by high molecular polymer monomer, linking agent, initiator, nano particle and long after glow luminous material Homogeneous phase mixing, obtain mixture;
Step 2: said mixture is uniformly coated on substrate surface, polymerization, obtains super-hydrophobic self-luminous coating.
Preferably, described high molecular polymer monomer is the one in polydimethylsiloxane, polymeric amide PA, polyethylene terephtalate, polyvinylchloride, polycarbonate, polystyrene PS, ethylene-vinyl acetate copolymer EVA, polyethylene octene elastic composite POE, polythene PE, polymetylmethacrylate, polyurethane PU, polypropylene PP or derivatives thereof;
Described linking agent is the one in aminoresin, acrylic amide, imines class, epoxy compounds class, silicone coupling agents, isocyanic ester;
Described initiator is light trigger or thermal initiator;
Described nano particle is nano-oxide, nano composite oxide or nano metal and alloy;
Described long after glow luminous material is the one in rare-earth sulfide long-lasting phosphor, rare earth silicate long-lasting phosphor or rare earth aluminate long-lasting phosphor;
Described base material is the one in glass, silicon chip, timber, metal, pottery, rubber, fabric, buildings.
Preferably, described light trigger is the one in radical polymerization light trigger or Cationic photoinitiator, and described thermal initiator is the one in peroxide, azo-initiator.
Preferably, the emission wavelength of described long after glow luminous material is within the scope of 400 ~ 800nm; In mixture prepared by described step 1, the mass content of long after glow luminous material is 5% ~ 30%.
Preferably, the ratio of described high molecular polymer monomer and initiator is 1: 1 ~ 20: 1, and in mixture prepared by described step 1, the content of linking agent is 0.1wt% ~ 5wt%.
Preferably, described nano particle comprises inorganic nanoparticles silicon-dioxide, titanium dioxide, silver, ferric oxide, tindioxide, silicon carbide, tetrafluoroethylene particulate, carbon, zirconium dioxide.
Preferably, the particle size range of described nano particle is 10 ~ 200nm; The concentration range of described nano particle is 5% ~ 30%.
Preferably, method when described mixture is uniformly coated on substrate surface comprises coating method, pinch-band technic or template; Described coating method comprises a painting, spin coating, roller coat, blade coating or brushing, and the speed of spin coating is 0.1 ~ 10.0kr/min, and the pressure of roller coat is 1 ~ 100N, and the speed of blade coating is 1 ~ 99mm/s, and dripping the volume be coated with is 1 ~ 100ml; The spacing thickness of described template and pinch-band technic is 10 ~ 1000 μm.
Preferably, in described step 2, the condition of polymerization is: heating induction is polymerized or passes through to cause rayed; Type of heating is place 1 ~ 5h at 60 ~ 120 DEG C; Causing light is the ultraviolet region of wavelength 250 ~ 420nm or the visible region of wavelength 400 ~ 800nm, and light application time 1 ~ 30 minute, intensity of illumination is 1mW/cm 2~ 2W/cm 2.
Preferably, the thickness of described super-hydrophobic self-luminous coating is 10 ~ 1000 μm, and emission wavelength is 400 ~ 800nm.
The present invention by the long after glow luminous material of different emission scope is carried out high molecular polymer coated and doping, the super-hydrophobic self-luminous coating of different substrate materials consistency can be obtained.This coating not only has super-hydrophobic automatic cleaning performance, solve the problem that long after glow luminous material meets water unstable, and there is pervasive substrate compatibility, be applicable to different substrate materials surface, and can be applicable to various humidity or emergency lighting under harsh environmental conditions and instruction.Long after glow luminous material add the hydrophobicity not only increasing polymeric film, and there is long-persistence luminous performance.Under the irradiation of natural light, sunlight can be absorbed rapidly and discharge slowly.By changing kind and the ratio of dopant material, the luminescent film of different colours and application function can be obtained.
Method provided by the invention overcomes the deficiencies in the prior art, while extending the range of application of long after glow luminous material, solves the difficult problem that it meets water decomposition or luminous intensity reduction.Method technique of the present invention is simple, saved preparation cost, and universality is strong.
Accompanying drawing explanation
Fig. 1 is the super-hydrophobic effect of the coating prepared in embodiment 2;
Fig. 2 is the super-hydrophobic effect of the coating prepared in embodiment 3.
Embodiment
For making the present invention become apparent, hereby with several preferred embodiment, be described in detail below.
Embodiment 1
Be that the long-lasting phosphor of blue (peak value is 456nm) adds in the mixture of 1g PMMA polymer monomer and initiator 2-hydroxy-2-methyl-to hydroxyethyl ether phenyl-acetone (ratio of monomer and initiator is 20: 1) by 0.05g utilizing emitted light, and add the linking agent vinyltriethoxysilane (VTES) that mass content is 0.1%, mass content is 5% hydrophobic Nano particles of silicon dioxide (particle size range is 10nm ~ 100nm), Keep agitation is until long-lasting phosphor and monomer, nano particle mixes, spread coating is adopted to drip on the glass sheet by said mixture, use coating machine even spread, surface covered is 99mm/s, then 1min is irradiated under the UV-light in 250 ~ 420nm wavelength region, light intensity magnitude is 1mW, prepare the super-hydrophobic luminescent coating of 10 μm of thick bluenesss, water droplet static contact angle is on the coating layer about 155 °.
Embodiment 2
Be that the long-lasting phosphor of green (peak value is 510nm) adds in the mixture of 25g PA high molecular polymer monomer and water-based azo initiator azo diisobutyl amidine hydrochloride (ratio of monomer and initiator is 10: 1) by 2.5g utilizing emitted light, and add the linking agent resol that mass content is 1%, mass content is the titanium dioxide nano-particle (particle size range is 10nm ~ 200nm) of 30%, Keep agitation is until mixture mixes, spread coating is adopted to drop on silicon chip by said mixture, use coating machine even spread, surface covered is 1mm/s, then at 120 DEG C, place 1h dry, obtain the PA film-green super-hydrophobic self-luminous coating of 1000 μm of thick doping long-lasting phosphors.As shown in Figure 1, preparation-obtained self-luminous coating as stated above, the water droplet contact angle recorded with static contact angle is 150 °.
Embodiment 3
Be that the long-lasting phosphor of red (peak value is 780nm) adds (ratio of monomer and initiator is 1: 1) in the mixture of 5g PET monomer and initiator benzophenone (DP) by 3g utilizing emitted light, and add the linking agent N that mass content is 5%, N '-methylene-bisacrylamide, mass content is the tin dioxide nano-particle (particle size range is 10nm ~ 200nm) of 30%, Keep agitation is until mixture mixes, adopt spin-coating method: dropped in by said mixture on plank base material, with the even spin coating of sol evenning machine, spin speed is 1kr/min, then 5min is irradiated under the UV-light in 250 ~ 420nm wavelength region, light intensity magnitude is 2W, obtain the super hydrophobic surface that thickness is the PET film-redness of 100 μm, as shown in Figure 2, preparation-obtained self-luminous coating as stated above, 153 ° are reached with the water droplet contact angle that static contact angle records.
Embodiment 4
Be that the long-lasting phosphor of blue (peak value is 456nm) adds (ratio of monomer and initiator is 1: 1) in the mixture of 1g PVC monomer and initiator Diisopropyl azodicarboxylate by 1g utilizing emitted light, and add the linking agent 2-n-butyl amine base-4 that mass content is 0.5%, 6-bis-dredges base s-triazine, mass content is the nanometer silicon carbide particle (particle size range is 50nm ~ 200nm) of 10%, and Keep agitation is until mixture mixes; Adopt spin-coating method: dropped in by said mixture on metal aluminium flake, with the even spin coating of desk-top sol evenning machine, spin speed is 10kr/min, then 1min is irradiated under the UV-light in 250 ~ 420nm wavelength region, light intensity magnitude is 2W, obtain the super-hydrophobic luminescent coating that thickness is the PVC film-blueness of 10 μm, preparation-obtained self-luminous coating as stated above, reaches 155 ° with the water droplet contact angle that static contact angle records.
Embodiment 5
Be that the long-lasting phosphor of red (peak value is 780nm) adds (ratio of monomer and initiator is 10: 1) in the mixture of 1g PC monomer and initiator di-cyclohexylperoxy dicarbonate by 0.1g utilizing emitted light, and mass content is the linking agent PMMA of 1%, mass content is the polytetrafluorethylenano nano particle (particle size range is 50nm ~ 200nm) of 15%, Keep agitation is until said mixture mixes, spread coating is adopted to drop on ceramic plate by said mixture, with the even roller coat of glass stick, pressure size is for being 10N, then at 80 DEG C, place 3h dry, obtain the super-hydrophobic self-luminous coating that thickness is the PC film-redness of 1 μm, 150 ° are greater than with the contact angle of light-emitting area.
Embodiment 6
Be that the long-lasting phosphor of green (peak value is 510nm) adds (ratio of monomer and initiator is 20: 1) in the mixture of 25g PA monomer and initiator di-isopropyl peroxydicarbonate by 7.5g utilizing emitted light, and mass content is the linking agent carbodiimide cross-linker of 5%, mass content is the Nano silver grain (particle size range is 10nm ~ 100nm) of 30%, Keep agitation is until long-lasting phosphor mixes, spread coating is adopted to drop on sheet rubber by said mixture, with the even roller coat of glass stick, pressure size is 0.1N, then at 120 DEG C, place 1h dry, obtain the super-hydrophobic luminescent coating that thickness is the PA film-green of 1000 μm.152 ° are about with the contact angle of light-emitting area.
Embodiment 7
Be that the long-lasting phosphor of red (peak value is 780nm) adds (ratio of monomer and initiator is 10: 1) in the mixture of 10g PE monomer and initiator dicumyl peroxide (DCP) by 2.5g utilizing emitted light, and mass content is the linking agent vinyl triethoxyl silicon burning of 0.5%, mass content is the ferric oxide nano particles (particle size range is 10nm ~ 200nm) of 30%, Keep agitation is until long-lasting phosphor mixes, then with pinch-band technic confinement preparation on silicon chip, the distance controlled between intermediate plate is 500 μm, then at 60 DEG C, place 5h dry, prepare the super-hydrophobic luminescent coating that thickness is the PE film-redness of 500 μm.155 ° are about with the contact angle of light-emitting area.
Embodiment 8
Be that the long-lasting phosphor of green (peak value is 510nm) adds (ratio of monomer and initiator is 1: 1) in the mixture of 1g PDMS monomer and initiator Diisopropyl azodicarboxylate by 0.1g utilizing emitted light, and mass content is that the vinylbenzene of 0.1% is as linking agent, mass content is the carbon nano-particles (particle size range is 10nm ~ 200nm) of 20%, Keep agitation is until long-lasting phosphor mixes, then groove depth monomer being added well in advance is in the mould of 10 μm, at 60 DEG C, place 5h dry, prepare the super-hydrophobic luminescent coating that thickness is the PDMS film-green of 10 μm.152 ° are about with the contact angle of light-emitting area.
Embodiment 9
Be that the long-lasting phosphor of red (peak value is 780nm) adds (ratio of monomer and initiator is 1: 1) in the mixture of 10g PET monomer and initiator Diisopropyl azodicarboxylate initiator by 0.05g utilizing emitted light, and mass content is the linking agent vinylchlorid of 0.5%, mass content is the Nano particles of silicon dioxide of 30% and the mixture (particle size range is 10nm ~ 200nm) of silicon carbide, Keep agitation is until said mixture mixes, then groove depth monomer being added well in advance is in the mould of 100 μm, at 120 DEG C, place 2h dry, prepare the super-hydrophobic luminescent coating that thickness is the PT film-redness of 100 μm.151 ° are about with the contact angle of light-emitting area.
Embodiment 10
Be that the long-lasting phosphor of green (peak value is 510nm) adds in 20g POE monomer and the luxuriant mixture of initiator fluorinated diphenyl titanium (ratio of monomer and initiator is 20: 1) by 6g utilizing emitted light, and mass content is the linking agent carbodiimide of 0.1%, mass content is titanium dioxide nano-particle and the nano SiO 2 particle mixture (particle size range is 10nm ~ 200nm) of 20%, Keep agitation is until long-lasting phosphor mixes, then groove depth monomer being added well in advance is in the mould of 1000 μm, then 30min is irradiated under the visible ray in 400 ~ 800nm wavelength region, light intensity magnitude is 2W, prepare the super-hydrophobic luminescent coating that thickness is the PT film-green of 1000 μm.156 ° are about with the contact angle of light-emitting area.
Embodiment 11
Be that the long-lasting phosphor of red (peak value is 780nm) adds in 15g PU monomer and the luxuriant mixture of two (pentafluorophenyl group) titanium of initiator (ratio of monomer and initiator is 10: 1) by 5g utilizing emitted light, and mass content is the linking agent polyoxyethylene of 5%, mass content is the polytetrafluorethylenano nano particle of 10% and the mixture (particle size range is 10nm ~ 200nm) of carbon nano-particle, Keep agitation is until long-lasting phosphor mixes, then groove depth monomer being added well in advance is in the mould of 500 μm, then 30min is irradiated under the visible ray in 400 ~ 800nm wavelength region, light intensity magnitude is 1W, prepare the super-hydrophobic luminescent coating that thickness is the PU film-redness of 500 μm.151 ° are about with the contact angle of light-emitting area.
Embodiment 12
Be that the long-lasting phosphor of green (peak value is 510nm) adds (ratio of monomer and initiator is 20: 1) in the mixture of 7g PP monomer and initiator di-t-butyl peroxide by 3g utilizing emitted light, and mass content is the linking agent PMMA of 0.1%, mass content is the ferriferrous oxide nano-particle (particle size range is 10nm ~ 200nm) of 5%, Keep agitation is until long-lasting phosphor mixes, spread coating is adopted to drop on sheet rubber by said mixture, with the even roller coat of glass stick, pressure size is for being 1N, then at 120 DEG C, place 1h dry, obtain the super-hydrophobic luminescent coating that thickness is the PS film-green of 200 μm.152 ° are about with the contact angle of light-emitting area.
Embodiment 13
Be that the long-lasting phosphor of green (peak value is 510nm) adds (ratio of monomer and initiator is 1: 1) in the mixing solutions of 1g EVA monomer and initiator 1-hydroxycyclohexyl phenyl ketone by 0.5g utilizing emitted light, and mass content be 0.1% linking agent gather dially phthalate, mass content is the zirconium dioxide nanoparticles (particle size range is 10nm ~ 200nm) of 30%, Keep agitation is until long-lasting phosphor mixes, adopting pinch-band technic mixture to be added thickness is in the intermediate plate of 10 μm, adopt ultraviolet region (250 ~ 420nm) for causing light, light application time is 2 minutes, intensity of illumination is 1mW/cm 2, prepare the super-hydrophobic luminescent coating that thickness is the PU film-green of 10 μm.152 ° are about with the contact angle of light-emitting area.

Claims (10)

1. a preparation method for super-hydrophobic self-luminous coating, is characterized in that: the method is made up of following 2 steps:
Step 1: by high molecular polymer monomer, linking agent, initiator, nano particle and long after glow luminous material Homogeneous phase mixing, obtain mixture;
Step 2: said mixture is uniformly coated on substrate surface, polymerization, obtains super-hydrophobic self-luminous coating.
2. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that:
Described high molecular polymer monomer is the one in polydimethylsiloxane, polymeric amide PA, polyethylene terephtalate, polyvinylchloride, polycarbonate, polystyrene PS, ethylene-vinyl acetate copolymer EVA, polyethylene octene elastic composite POE, polythene PE, polymetylmethacrylate, polyurethane PU, polypropylene PP or derivatives thereof;
Described linking agent is the one in aminoresin, acrylic amide, imines class, epoxy compounds class, silicone coupling agents, isocyanic ester;
Described initiator is light trigger or thermal initiator;
Described nano particle is nano-oxide, nano composite oxide or nano metal and alloy;
Described long after glow luminous material is the one in rare-earth sulfide long-lasting phosphor, rare earth silicate long-lasting phosphor or rare earth aluminate long-lasting phosphor;
Described base material is the one in glass, silicon chip, timber, metal, pottery, rubber, fabric, buildings.
3. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 2, it is characterized in that: described light trigger is the one in radical polymerization light trigger or Cationic photoinitiator, and described thermal initiator is the one in peroxide, azo-initiator.
4. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: the emission wavelength of described long after glow luminous material is within the scope of 400 ~ 800nm; In mixture prepared by described step 1, the mass content of long after glow luminous material is 5% ~ 30%.
5. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: the ratio of described high molecular polymer monomer and initiator is 1: 1 ~ 20: 1, and in mixture prepared by described step 1, the content of linking agent is 0.1wt% ~ 5wt%.
6. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, it is characterized in that: described nano particle comprises inorganic nanoparticles silicon-dioxide, titanium dioxide, silver, ferric oxide, tindioxide, silicon carbide, tetrafluoroethylene particulate, carbon, zirconium dioxide.
7. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: the mass content of described nano particle is 5% ~ 30%, and size is 10nm ~ 200nm.
8. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: method when described mixture is uniformly coated on substrate surface comprises coating method, pinch-band technic or template; Described coating method comprises a painting, spin coating, roller coat, blade coating or brushing, and the speed of spin coating is 0.1 ~ 10.0kr/min, and the pressure of roller coat is 1 ~ 100N, and the speed of blade coating is 1 ~ 99mm/s, and dripping the volume be coated with is 1 ~ 100ml; The spacing thickness of described template and pinch-band technic is 10 ~ 1000 μm.
9. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: in described step 2, the condition of polymerization is: heating induction is polymerized or passes through to cause rayed; Type of heating is place 1 ~ 5h at 60 ~ 120 DEG C; Causing light is the ultraviolet region of wavelength 250 ~ 420nm or the visible region of wavelength 400 ~ 800nm, and light application time 1 ~ 30 minute, intensity of illumination is 1mW/cm2 ~ 2W/cm2.
10. the preparation method of super-hydrophobic self-luminous coating as claimed in claim 1, is characterized in that: the thickness of described super-hydrophobic self-luminous coating is 10 ~ 1000 μm, and emission wavelength is 400 ~ 800nm.
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