CN103387787A - Organic/inorganic hybrid transparent heat-insulating coating material, and preparation method and application thereof - Google Patents
Organic/inorganic hybrid transparent heat-insulating coating material, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an organic/inorganic hybrid transparent heat-insulating coating material. The coating material comprises the following raw materials by mass: 45 to 85 parts of a UV light-cured resin, 5 to 50 parts of a nanometer heat-insulating particle dispersion liquid and 1 to 4 parts of an auxiliary agent. The invention also discloses a preparation method for the coating material. The preparation method comprises the following steps: (1) preparation of the nanometer heat-insulating particle dispersion liquid; (2) preparation of a nanometer modified sol; (3) preparation of the organic/inorganic hybrid UV-cured resin; and (4) preparation of the hybrid transparent heat-insulating coating material: a step of preparing the raw materials according to above-mentioned mass proportions, adding the raw materials into a reaction vessel and carrying out high speed dispersion so as to obtain the coating material. The invention further discloses application of the coating material. The coating material is applicable to heat insulation and protection in the aspects of energy-saving electric light sources, photoelectric materials, energy-saving windows, solar cells, etc. According to the invention, through addition of a functional heat-insulating particle into an organic/inorganic hybrid resin system, an obtained transparent heat-insulating coating has high visible light transmittance and a substantial effect on obstruction of infrared and near infrared heat radiation.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to the transparent heat-insulated coated material of a kind of hybrid for surface of polymer substrates, preparation method and application thereof; This coating has sticking power and visible light transmissivity well at the plastic polymer substrate surface, to infrared obvious with near infrared light thermal radiation barriering effect;
Background technology
Heat insulating coat is a kind of functional coats heat insulation, sun-proof, energy-saving and environmental protection that have.Infrared thermal reflective coating is the heat insulating coat of applying early, it has high-reflectivity and high emissivity, by the selective reflection ir radiation, stop transmission, the inhibition heat deposition of heat from source, reduce and be exposed to surface temperature and the interior environment temperature of equipping under sun heat radiation.Thereby reach the effect of heat insulating.
Heat insulating coat has been successfully applied to the fields such as building roof and glass curtain wall, offshore drilling platform, petroleum pipe line, aircraft, warship, rocket abroad.Domestic research report aspect heat preserving and insulating material is more, as CN102766366A, adopts silicon emulsion, hollow glass bead, titanium dioxide etc. to be mixed with a kind of reflective heat-insulation paint.This coating has reflection and diffraction well to sunlight, and intercept heat enters matrix inside.Thereby acquisition effect of heat insulation.CN101235243A discloses a kind of multifunctional coating with heat reflection and heat rejection.This coating is comprised of thermosetting resin, Rutile type Titanium Dioxide and functional stuffing.The coating that obtains has high-reflectivity to visible light and near infrared light, has in 8/13.5 mu m waveband that severe radiation rate, low heat conductivity, cooling-down effect are good, camouflage effectiveness and characteristics such as antiseptic property is good.But these coatings often all have opacity, and heat-insulating property is poor.And base material there is strict requirement.Limited its range of application.
Along with the application of heat insulating coat in field of photovoltaic materials, the research of transparent heat-insulated coating becomes focus.Require it optionally to see through visible light, simultaneously ir radiation is had very high rejection rate.Patent WO2005059013A1 discloses a kind of polymer thin membrane preparation method of blocking infrared transmission.This invention with functional particles ITO grinding distribution to polyvinyl butyral acetal and Dimethylformamide, the infrared barrier printing ink of acquisition by mode of printing to glass surface.This coating has good adhesive property and photo-thermal barrier properties to glass.CN 101792636A discloses the aqueous heat-insulating nano composite coating material that a kind of UV solidifies.The film that obtains through curing has good transparency and heat-proof quality, and this thermal insulation protection coating can be applicable to the aspects such as automotive window, glass of building curtain wall.
At present, the transparent heat-insulated coating overwhelming majority is applied to the glass baseplate surface, and application rarely has report on polymer surfaces.This is that while because of conventional organic resin, being coated on pliable and tough polymer surfaces, its sticking power and mechanical property are undesirable.Cause its over-all properties and work-ing life to descend.Introduce the organic/inorganic nano composite coating technology and can effectively overcome the problems referred to above.It can solve the requirement of coating to sticking power and mechanical property as film-forming resin.Visible light transmissivity is high, to infrared obvious with near infrared light thermal radiation barriering effect.Can be used for the fields such as energy-conserving light source, Energy Saving Windows, photoelectric material and solar cell.
Summary of the invention
For the prior art above shortcomings, the object of the present invention is to provide material of a kind of transparent heat-insulated coating of hybrid that can be used for surface of polymer substrates and preparation method thereof, this coated material preparation technology rationally, be easy to control, environmentally friendly, the coating machine performance is good, hardness is high, and polymeric substrate is had sticking power well.
The present invention also provides the application of this heat-proof coating material.
The technical scheme that the present invention adopts for achieving the above object is:
The transparent heat-insulated coated material of a kind of hybrid, its raw material by following mass fraction forms:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is one of AFCONA dispersion agent, AFCONA flow agent or its mixture.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
The preparation method of the hybrid transparent heat-insulated coated material above-mentioned according to preparation, it comprises the steps:
(1) prepare the nano heat-insulating particle dispersion:
, with functional particles and the Virahol ratio of 1: 2 in mass ratio～1: 6, join in dispersion cup; Then add 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) account for functional particles and Virahol quality summation, under the rotating speed of 1500～3000r/min, Ball milling 1～6h; Namely obtain stably dispersing, the uniform nano heat-insulating particle dispersion of size distribution;
(2) prepare nano modification colloidal sol:
(21) described nano modification colloidal sol, its raw material by following component is made, and according to the mass fraction of each following feed composition, prepares each feed composition:
(22) Nano sol and silane coupling agent are added in reactor by above-mentioned mass fraction, after stirring, more slowly drip the aqueous acetic acid that is made into according to above-mentioned mass fraction by acetic acid and deionized water, stirring reaction 2～8 hours, ageing 24 hours, get final product to obtain nano modification colloidal sol;
(3) prepare hybrid UV cured resin:
(31) prepare each feed composition according to following mass ratio:
(32) nano modification colloidal sol, UV cured resin, light trigger and dispersion agent are mixed to join in dispersion cup by above-mentioned mass fraction, disperse to stir 0.5～3h, get final product to obtain hybrid UV cured resin;
(4) organic/inorganic hybrid transparent heat-proof coating material of preparation:
(41) prepare raw material according to following mass ratio:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
(42) with hybrid UV light-cured resin, nano heat-insulating particle dispersion and auxiliary agent, mix and add in reactor according to above-mentioned mass fraction, under the rotating speed of 2000～3000r/min, high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid.
Described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
Described Nano sol is one or more combinations in TiO 2 sol, aluminium sesquioxide colloidal sol, silicon dioxide gel, zirconia sol.
Described silane coupling agent is one or more combinations in γ-methacryloxypropyl trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyl triethoxysilane, vinyltriethoxysilane, allyl trimethyl silane and vinyltrimethoxy silane.
Described UV cured resin comprises one or more combinations in epoxy acrylate oligomer, polyurethane acrylic ester oligomer, polyester acrylic ester oligomer, aminoacrylic acid ester oligomer, pure acrylic acid fat oligopolymer, unsaturated polyester ester oligomer, polyoxytrimethylene acid polyvalent alcohol oligopolymer and phosphorus modified acroleic acid ester oligomer.
A kind of application of the above-mentioned transparent heat-insulated coated material of hybrid, it is for the preparation of the coating of surface of polymer substrates, and the visible light transmittance rate of this coating 〉=88%, to infrared and near infrared light thermal radiation rejection rate 〉=80%.
Described polymeric substrate is a kind of in polymethylmethacrylate (PMMA), polycarbonate (PC), acrylonitrile/butadiene/styrene plastics (ABS) and polyethylene terephthalate (PET).
Beneficial effect of the present invention is: material provided by the invention and method, by the hybrid composite coating technology being introduced the preparation of heat-insulation transparent coating, add modified function colloidal sol to make coating have satisfactory stability, wear resistance and scratch resistance, give the transparency of this coated material excellence, simultaneously, the hybrid heat-proof coating material has good sticking power at polymer surfaces; The present invention is by adding functional insulation particle to the hybrid resin system; the transparent heat-insulated coating visible light transmissivity that obtains is high; to infrared obvious with near infrared light thermal radiation barriering effect, product can be widely used in the thermal insulation protection of the aspects such as energy-saving electric light source, Energy Saving Windows, automobile frost shield and solar cell.
Embodiment
Embodiment 1:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is one of AFCONA dispersion agent, AFCONA flow agent or its mixture, and the visual particular case of its blending ratio is determined according to known technology.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
Prepare the preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) prepare the nano heat-insulating particle dispersion:
, with functional particles and the Virahol ratio of 1: 2 in mass ratio～1: 6, join in dispersion cup; Then add 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) account for functional particles and Virahol quality summation, under the rotating speed of 1500～3000r/min, Ball milling 1～6h; Namely obtain stably dispersing, the uniform nano heat-insulating particle dispersion of size distribution;
(2) prepare nano modification colloidal sol:
(21) described nano modification colloidal sol, its raw material by following component is made, and according to the mass fraction of each following feed composition, prepares each feed composition:
(22) Nano sol and silane coupling agent are added in reactor by above-mentioned mass fraction, after stirring, more slowly drip the aqueous acetic acid that is made into according to above-mentioned mass fraction by acetic acid and deionized water, stirring reaction 2～8 hours, ageing 24 hours, get final product to obtain nano modification colloidal sol;
(3) prepare hybrid UV cured resin:
(31) prepare each feed composition according to following mass ratio:
(32) nano modification colloidal sol, UV cured resin, light trigger and dispersion agent are mixed to join in dispersion cup by above-mentioned mass fraction, disperse to stir 0.5～3h, get final product to obtain hybrid UV cured resin;
(4) organic/inorganic hybrid transparent heat-proof coating material of preparation:
(41) prepare raw material according to following mass ratio:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
(42) with hybrid UV light-cured resin, nano heat-insulating particle dispersion and auxiliary agent, mix and add in reactor according to above-mentioned mass fraction, under the rotating speed of 2000～3000r/min, high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid.
Described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
Described Nano sol is one or more combinations in TiO 2 sol, aluminium sesquioxide colloidal sol, silicon dioxide gel, zirconia sol.
Described silane coupling agent is one or more combinations in γ-methacryloxypropyl trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyl triethoxysilane, vinyltriethoxysilane, allyl trimethyl silane and vinyltrimethoxy silane.
Described UV cured resin comprises one or more combinations in epoxy acrylate oligomer, polyurethane acrylic ester oligomer, polyester acrylic ester oligomer, aminoacrylic acid ester oligomer, pure acrylic acid fat oligopolymer, unsaturated polyester ester oligomer, polyoxytrimethylene acid polyvalent alcohol oligopolymer and phosphorus modified acroleic acid ester oligomer.
A kind of application of the above-mentioned transparent heat-insulated coated material of hybrid, it is for the preparation of the coating of surface of polymer substrates, and the visible light transmittance rate of this coating 〉=88%, to infrared and near infrared light thermal radiation rejection rate 〉=80%.
Described polymeric substrate is a kind of in polymethylmethacrylate (PMMA), polycarbonate (PC), acrylonitrile/butadiene/styrene plastics (ABS) and polyethylene terephthalate (PET).
Embodiment 2:
Transparent heat-insulated coated material of hybrid that is used for surface of polymer substrates that the present embodiment provides and preparation method thereof, application, it is substantially the same manner as Example 1, and its difference is:
The transparent heat-insulated coated material of the hybrid that the present embodiment provides, its raw material by following mass fraction forms:
84 parts of hybrid UV light-cured resins
14 parts of nano heat-insulating particle dispersions
2 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is the mixture of AFCONA dispersion agent, AFCONA, and its blending ratio is 1: 1wt.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano oxidized antimony tin (ATO).
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take 14g nano ATO particle, 32.3g Virahol and 0.4g polyethylene of dispersing agent pyrrolidone, then join in dispersion cup, adopt the Ball milling method, Ball milling 6h under the 1600r/min rotating speed, obtain stably dispersing PVP, the uniform nano ATO dispersion liquid of size distribution;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 28.5g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.6g acetic acid and 14.5 deionized waters are made into, dropwise in 45min, continue stirring reaction 2-8 hour, ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent;
(3) preparation of hybrid UV cured resin
Nano modification silicon sol 27.8g, polyurethane acrylic ester oligomer 8.3g, epoxy acrylate oligomer 6.2g, Viscoat 295 4.2g, light trigger 0.9g and dispersion agent 0.7g that step (2) is obtained are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain organic/inorganic UV cured resin.
(4) preparation of the transparent heat-insulated coated material of hybrid
Step (1) gained nano ATO dispersion liquid 7.5g, step (3) gained organic/inorganic UV cured resin 45g and auxiliary agent 1.1g are mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
Embodiment 3:
Transparent heat-insulated coated material of hybrid that is used for surface of polymer substrates that the present embodiment provides and preparation method thereof, application, itself and embodiment 1 or 2 are basic identical, and its difference is:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
76.7 parts of hybrid UV light-cured resins
21.3 parts of nano heat-insulating particle dispersions
2.0 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is the AFCONA dispersion agent.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano titanium oxide (TiO
2).
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take 14g nano titanium oxide (TiO
2) particle, 32.3g Virahol and 0.4g polyethylene of dispersing agent pyrrolidone, then join in dispersion cup, adopt the Ball milling method, Ball milling 6h under the 1600r/min rotating speed, obtain stably dispersing PVP, the uniform nano titanium dioxide of size distribution (TiO
2) dispersion liquid;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 28.5g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.6g acetic acid and 14.5 deionized waters are made into, dropwise in 45min, continue stirring reaction 2-8 hour, ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent;
(3) preparation of hybrid UV cured resin
Nano modification silicon sol 27.8g, polyurethane acrylic ester oligomer 8.3g, epoxy acrylate oligomer 6.2g, Viscoat 295 4.2g, light trigger 0.9g and dispersion agent 0.7g that step (2) is obtained are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain organic/inorganic UV cured resin.
(4) preparation of the transparent heat-insulated coated material of hybrid
With step (1) gained nano titanium oxide (TiO
2) dispersion liquid 12.5g, step (3) gained hybrid UV cured resin 45g and auxiliary agent 1.2g be mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
Embodiment 4:
Transparent heat-insulated coated material of hybrid that is used for surface of polymer substrates that the present embodiment provides and preparation method thereof and application, itself and embodiment 1,2,3 basic identical, its difference is:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
70.6 parts of hybrid UV light-cured resins
27.4 parts of nano heat-insulating particle dispersions
2 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is the AFCONA flow agent.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano zine oxide (ZnO).
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take 14g nano zine oxide (ZnO) particle, 32.3g Virahol and 0.4g polyethylene of dispersing agent pyrrolidone, then join in dispersion cup, adopt the Ball milling method, Ball milling 6h under the 1600r/min rotating speed, obtain stably dispersing PVP, the uniform nano zine oxide of size distribution (ZnO) dispersion liquid;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 28.5g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.6g acetic acid and 14.5 deionized waters are made into, dropwise in 45min, continue stirring reaction 2-8 hour, ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent;
(3) preparation of hybrid UV cured resin
Nano modification silicon sol 27.8g, polyurethane acrylic ester oligomer 8.3g, epoxy acrylate oligomer 6.2g, Viscoat 295 4.2g, light trigger 0.9g and dispersion agent 0.7g that step (2) is obtained are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain organic/inorganic UV cured resin.
(4) preparation of the transparent heat-insulated coated material of hybrid
Step (1) gained nano zine oxide (ZnO) dispersion liquid 17.5g, step (3) gained hybrid UV cured resin 45g and auxiliary agent 1.3g are mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
Embodiment 5:
Transparent heat-insulated coated material of hybrid that is used for surface of polymer substrates that the present embodiment provides and preparation method thereof and application, itself and embodiment 1,2,3,4 basic identical, its difference is:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
65.3 parts of hybrid UV light-cured resins
32.7 parts of nano heat-insulating particle dispersions
2 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is AFCONA dispersion agent and AFCONA flow agent.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is nano aluminium oxide (Al
2O
3).
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take 14g nano aluminum oxide (Al
2O
3) particle, 32.3g Virahol and 0.4g polyethylene of dispersing agent pyrrolidone, then join in dispersion cup, adopt the Ball milling method, Ball milling 6h under the 1600r/min rotating speed, obtain stably dispersing PVP, the uniform nano aluminium oxide (Al of size distribution
2O
3) dispersion liquid;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 28.5g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.6g acetic acid and 14.5 deionized waters are made into, dropwise in 45min, continue stirring reaction 2-8 hour, ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent;
(3) preparation of hybrid UV cured resin
Nano modification silicon sol 27.8g, polyurethane acrylic ester oligomer 8.3g, epoxy acrylate oligomer 6.2g, Viscoat 295 4.2g, light trigger 0.9g and dispersion agent 0.7g that step (2) is obtained are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain organic/inorganic UV cured resin.
(4) preparation of the transparent heat-insulated coated material of hybrid
With step (1) gained nano aluminium oxide (Al
2O
3) dispersion liquid 22.5g, step (3) gained hybrid UV cured resin 45g and auxiliary agent 1.4g be mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
Embodiment 6:
The preparation method of the transparent heat-insulated coated material of hybrid that is used for surface of polymer substrates that the present embodiment provides, its step and embodiment 1,2,3,4,5 basic identical, its difference is:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
65.3 parts of hybrid UV light-cured resins
32.7 parts of nano heat-insulating particle dispersions
2 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is AFCONA dispersion agent and AFCONA flow agent.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is mica powder.
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take 14g mica powder, 55.6g Virahol and 0.4g polyethylene of dispersing agent pyrrolidone (PVP), then join in dispersion cup, adopt the Ball milling method, Ball milling 4h under the 2000r/min rotating speed, obtain stably dispersing, the uniform mica powder dispersion liquid of size distribution;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 42.8g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.9g acetic acid and 17.1 deionized waters are made into, dropwise in 45min, continued stirring reaction 2/8 hour.Ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent;
(3) preparation of hybrid UV cured resin;
Nano modification silicon sol 35.5g and polyurethane acrylic ester oligomer 10.6g, epoxy acrylate oligomer 8.0g, Viscoat 295 5.3g, light trigger 1.2g and dispersion agent 0.9g that step (2) is obtained are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain hybrid UV cured resin;
(4) preparation of the transparent heat-insulated coated material of hybrid
Step (1) gained mica powder dispersion liquid 22.5g, step (3) gained hybrid UV cured resin 45g and auxiliary agent 1.4g are mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
Embodiment 7:
The transparent heat-insulated coated material of hybrid, preparation method and the application thereof that are used for surface of polymer substrates that the present embodiment provides, its step and embodiment 1,2,3,4,5,6 basic identical, its difference is:
The transparent heat-insulated coated material of hybrid provided by the invention, its raw material by following mass fraction forms:
65.3 parts of hybrid UV light-cured resins
32.7 parts of nano heat-insulating particle dispersions
2 parts of auxiliary agents;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is AFCONA dispersion agent and AFCONA flow agent.
Wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
Wherein, described functional particles is high-purity light reflecting material YZ.
The preparation method of the above-mentioned transparent heat-insulated coated material of hybrid, it comprises the steps:
(1) preparation of nano heat-insulating particle dispersion
Take the high-purity light reflecting material YZ of 9.5g, 29.4g Virahol and 0.3g polyethylene of dispersing agent pyrrolidone (PVP), then join in dispersion cup, adopt the Ball milling method, Ball milling 4h under the 2000r/min rotating speed, obtain stably dispersing, the uniform high-purity light reflecting material YZ dispersion liquid of size distribution;
(2) preparation of nano modification colloidal sol
The Nano silica sol of 51.8g solid content 20% and 28.5g silane coupling agent γ-methacryloxypropyl trimethoxy silane are added in reactor, after stirring, slowly drip the aqueous acetic acid that 1.6g acetic acid and 14.5 deionized waters are made into, dropwise in 45min, continued stirring reaction 2/8 hour, ageing 24 hours, get final product to obtain the nano modification colloidal sol of this silane coupling agent.
(3) preparation of hybrid UV cured resin;
Nano modification silicon sol 27.8g, the polyurethane acrylic ester oligomer 11.0g, epoxy acrylate oligomer 8.2g, Viscoat 295 5.5g, light trigger 1.2g and the dispersion agent 0.8g that obtain in step (2) are mixed to join in dispersion cup, dispersed with stirring 30min, can obtain hybrid UV cured resin;
(4) preparation of the transparent heat-insulated coated material of hybrid
The high-purity light reflecting material YZ of step (1) gained dispersion liquid 22.5g, step (3) gained hybrid UV cured resin 45g and auxiliary agent 1.4g are mixed to join in reactor, at 2000r/min high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid, then be coated to surface of polymer substrates by spraying method, adopt the UV radiation curing, obtain the transparent heat-insulated coating of functional hybrid.
above-described embodiment has only been put down in writing several preferred versions, can also utilize one or more combinations in other functional particles of specification sheets or claims record to prepare the nano heat-insulating particle dispersion, simultaneously, also can utilize other one or more combinations of silane coupling agent of specification sheets or claims record to prepare nano modification colloidal sol, can utilize other one or more combinations of UV cured resin of specification sheets or claims record to prepare hybrid UV cured resin, therefore, also can utilize the different nano heat-insulating particle dispersion of above-mentioned preparation, hybrid UV cured resin prepares organic/inorganic hybrid transparent heat-proof coating material.
The salient features of the transparent heat-insulated coating of hybrid in embodiment 2～5 detects according to the concerned countries standard;
Concrete test result is as shown in following table:
Beneficial effect of the present invention is: the present invention introduces the preparation of heat-insulation transparent coating with the hybrid composite coating technology.Add modified function colloidal sol to make coating have satisfactory stability, wear resistance and scratch resistance.Give the transparency of coating excellence, simultaneously, the hybrid heat insulating coat has good sticking power at polymer surfaces.By adding functional insulation particle to the hybrid resin system, the transparent heat-insulated coating visible light transmissivity of acquisition is high, to infrared obvious with near infrared light thermal radiation barriering effect.
But the foregoing is only better possible embodiments of the present invention; not in order to limit to the scope of the claims of the present invention; therefore other embodiment of step, component and the application put down in writing in all utilization the present invention, and the equivalence of doing variation, all be included in protection scope of the present invention.
Claims (10)
1. the transparent heat-insulated coated material of hybrid, is characterized in that, its raw material by following mass fraction forms:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
Wherein, described hybrid UV light-cured resin is comprised of the raw material of following mass fraction:
Wherein, described nano heat-insulating particle dispersion is to be functional particles and the Virahol of 1: 2～1: 6 by mass ratio, with 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) that accounts for functional particles and Virahol quality summation, makes;
Described auxiliary agent is one of AFCONA dispersion agent, AFCONA flow agent or its mixture.
2. the transparent heat-insulated coated material of hybrid according to claim 1, is characterized in that, wherein, nano modification colloidal sol, its raw material by following mass fraction forms:
3. the transparent heat-insulated coated material of hybrid according to claim 1, is characterized in that, wherein, described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
4. prepare the method for the transparent heat-insulated coated material of the described hybrid of one of claim 1～3, it is characterized in that: it comprises the steps:
(1) prepare the nano heat-insulating particle dispersion:
, with functional particles and the Virahol ratio of 1: 2 in mass ratio～1: 6, join in dispersion cup; Then add 0.5～5% the polyethylene of dispersing agent pyrrolidone (PVP) account for functional particles and Virahol quality summation, under the rotating speed of 1500～3000r/min, Ball milling 1～6h; Namely obtain stably dispersing, the uniform nano heat-insulating particle dispersion of size distribution;
(2) prepare nano modification colloidal sol:
(21) described nano modification colloidal sol, its raw material by following component is made, and according to the mass fraction of each following feed composition, prepares each feed composition:
(22) Nano sol and silane coupling agent are added in reactor by above-mentioned mass fraction, after stirring, more slowly drip the aqueous acetic acid that is made into according to above-mentioned mass fraction by acetic acid and deionized water, stirring reaction 2～8 hours, ageing 24 hours, get final product to obtain nano modification colloidal sol;
(3) prepare hybrid UV cured resin:
(31) prepare each feed composition according to following mass ratio:
(32) nano modification colloidal sol, UV cured resin, light trigger and dispersion agent are mixed to join in dispersion cup by above-mentioned mass fraction, disperse to stir 0.5～3h, get final product to obtain hybrid UV cured resin;
(4) organic/inorganic hybrid transparent heat-proof coating material of preparation:
(41) prepare raw material according to following mass ratio:
Hybrid UV light-cured resin 45-85 part
Nano heat-insulating particle dispersion 5-50 part
Auxiliary agent 1-4 part;
(42) with hybrid UV light-cured resin, nano heat-insulating particle dispersion and auxiliary agent, mix and add in reactor according to above-mentioned mass fraction, under the rotating speed of 2000～3000r/min, high speed dispersion 30min, can obtain the transparent heat-insulated coated material of hybrid.
5. the preparation method of the transparent heat-insulated coated material of hybrid according to claim 4, it is characterized in that: described functional particles is nano titanium oxide (TiO
2), nano zine oxide (ZnO), nano aluminium oxide (Al
2O
3), nano silicon (SiO
2), mica powder, talcum powder (Talc), high-purity light reflecting material YZ, nano oxidized zinc-aluminium, metal scale, ferriferous oxide, lanthanum hexaborane (LaB
6), one or more combinations in antimony tin (ATO), tin indium oxide (ITO), hollow ceramic particulate, inorganic fibre.
6. the preparation method of the transparent heat-insulated coated material of hybrid according to claim 4, it is characterized in that: described Nano sol is one or more combinations in TiO 2 sol, aluminium sesquioxide colloidal sol, silicon dioxide gel, zirconia sol.
7. the preparation method of the transparent heat-insulated coated material of hybrid according to claim 4, it is characterized in that: described silane coupling agent is one or more combinations in γ-methacryloxypropyl trimethoxy silane, γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-aminopropyl triethoxysilane, vinyltriethoxysilane, allyl trimethyl silane and vinyltrimethoxy silane.
8. the preparation method of the transparent heat-insulated coated material of hybrid according to claim 4 is characterized in that: described UV cured resin comprises one or more combinations in epoxy acrylate oligomer, polyurethane acrylic ester oligomer, polyester acrylic ester oligomer, aminoacrylic acid ester oligomer, pure acrylic acid fat oligopolymer, unsaturated polyester ester oligomer, polyoxytrimethylene acid polyvalent alcohol oligopolymer and phosphorus modified acroleic acid ester oligomer.
9. the application of one of according to claim 1～8 transparent heat-insulated coated materials of described hybrid, it is characterized in that, it is for the preparation of the coating of surface of polymer substrates, and the visible light transmittance rate of this coating 〉=88%, to infrared and near infrared light thermal radiation rejection rate 〉=80%.
10. the application of the transparent heat-insulated coated material of hybrid according to claim 9 is characterized in that: described polymeric substrate is a kind of in polymethylmethacrylate (PMMA), polycarbonate (PC), acrylonitrile/butadiene/styrene plastics (ABS) and polyethylene terephthalate (PET).
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