CN103980643A - Blue light cut nano compound resin material, lens and preparation method thereof - Google Patents
Blue light cut nano compound resin material, lens and preparation method thereof Download PDFInfo
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- CN103980643A CN103980643A CN201410245196.0A CN201410245196A CN103980643A CN 103980643 A CN103980643 A CN 103980643A CN 201410245196 A CN201410245196 A CN 201410245196A CN 103980643 A CN103980643 A CN 103980643A
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Abstract
The invention relates to a blue light cut nano compound resin material and lens and a manufacturing method thereof. The blue light cut nano compound resin material comprises macromolecule resin as well as core-shell type transition metal oxide nano particles and an ultraviolet light absorber which are dispersed in the macromolecule resin, wherein the core-shell type transition metal oxide nano particles account for 0.2-2% of the total weight of the resin, and the ultraviolet light absorber accounts for 0.5-5% of the total weight of the resin; particle size of nano particles is 20-50nm; the shell is a surface active agent, and thickness is 3-10nm; the nano particles and the ultraviolet light absorber are fully dispersed in a macromolecule monomer, and a prepolymerization and secondary polymerization technological process is carried out, so that the blue light cut compound resin material is obtained. The manufacturing method of the blue light cut compound resin material is simple in technology and good in reproducibility, the manufactured resin material and lens can efficiently and permanently shield high energy harmful blue light and ultraviolet light with wavelength within the range of 380-450nm, vision is clear and colour vision is soft under strong and weak light environments respectively, and the blue light cut compound resin material has excellent overall performance.
Description
Technical field
The present invention relates to a kind of optical material, eyeglass and preparation method thereof, especially a kind of anti-blue light nano-composite resin material, eyeglass and preparation method thereof.
Background technology
As everyone knows, ultraviolet ray has strong detrimental effect to eyes.Eyes long-term exposure, under ultraviolet ray, easily causes from cataract or glaucoma, causes retinal pigment epithelium damage, causes and even accelerates old maculopathy etc.In addition, there are some researches show, blue light (wavelength is the short wavelength light of 380-500nm scope) in visible ray can penetrate lens and arrive retina, retina can produce free radical through blue light long-term irradiation, and these free radicals can cause retinal pigment epithelium decline, and then cause photosensitive cell to lack nutrient, finally cause vision impairment.And its degree of damage increases sharply along with reducing of optical wavelength.The studied confirmation of blue light is the visible ray of tool harm.Medical research also shows, the purple light of human eye to 380-450nm wave band and part blue light depending on thing and distinguish that look insensitive, the color discrimination ability of the coloured light of eyes to this wave band is limited, but this band of light wave-wave length energy is high, larger to eye injury.Therefore, effectively avoid the following blue light of 450nm and ultraviolet irradiation most important to protection eyes.
Along with the progress and development of modern society, the products such as LED lamp, TV, computer display screen, smart mobile phone, panel computer have now been widely used in the every aspect of people's life, the high energy shortwave blue light that contains a large amount of irregular frequencies in the light that these products (especially LED lamp and display screen) send.Closely watch for a long time image, word, video etc., can cause certain pressure to eyes, and then occur blood-shot eye illness, eye is dry, and eye is puckery, blurred vision, asthenopia, the symptoms such as head, back, shoulder and cervical vertebra ache.Therefore, for long-term worker under indoor and outdoor high light environment, there is the working clan from patient, student family and the life-time service computer of cataract or glaucoma and maculopathy, wearing anti-blue light glasses is very necessary and the most simple and effective ways.
Present many anti-blue light resin lens are that organic staining agents such as melanochrome, yellow pigment are contaminated on doping or surface in eyeglass base material, utilize optical color in and principle reach certain blue light neutralization, filter effect.But, due to organic dye weathering resistance a little less than, can fade through sunlight long-term irradiation, can not be durable in use.In addition, the blue light percent of pass less than 10% of a lot of eyeglasses, pass through again thus lens and Vitrea further absorption in eyes, the blue light amount of wearing the real human eye retina of arrival after this high resistance blue light glasses is almost nil, namely intercept the blue coloured light in coloured light three primary colours (red, green, blue) completely, result can cause picture serious distortion, if things go on like this can reduce the color sense lightsensitivity of optic nerve, has the risk that causes anomalous trichromatism and even colour blindness.Moreover, coloured anti-blue light eyeglass is lower to the selectivity transmitance of long wave visible ray, while wearing, look thing and chromatic discrimination power a little less than, especially under cloudy day or low light environment, consistent effectively the improving one's methods that present stage takes is the even more multi-layered anti-reflection film of evaporation 3-11 layer, and manufacturing processed is numerous and diverse and antireflective effect is limited.Therefore, seek simple and effective manufacturing process, and then produce high-performance anti-blue light resin material, the eyeglass of excellent combination property, make it have high-efficient and lasting anti-blue light, all can be clear under strong and weak luminous environment depending on thing and distinguish the excellent properties that look soft, significant.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of anti-blue light nano-composite resin material, eyeglass and manufacture method thereof are provided, this manufacturing approach craft is simple, favorable reproducibility, can greatly improve industrial production efficiency; The resin material that makes, eyeglass energy high-efficient and lasting shielding wavelength be in the harmful blue light of high energy and the ultraviolet ray of 380-450nm scope, all can be clear under strong and weak luminous environment depending on thing and distinguish that look soft, over-all properties is good.
For achieving the above object, the present invention includes following technical scheme:
A kind of anti-blue light nano-composite resin material, this material comprises the macromolecule resin for making optical material and is scattered in hud typed transition metal oxide nano-particles and the UV light absorber of macromolecule resin; Wherein, hud typed transition metal oxide nano-particles accounts for the 0.2%-2% of total resin weight, and UV light absorber accounts for the 0.5%-5% of total resin weight.
Anti-blue light nano-composite resin material as above, preferably, described is to be polymerized by high polymer monomer for making the macromolecule resin of optical material, and this high polymer monomer is selected from: at least one in vinyl monomer, acrylate type monomer, allyl type monomer, epoxy resin high polymer monomer, polycarbonate-based high polymer monomer and polyurethane series high polymer monomer.More preferably, this high polymer monomer is selected from: at least one in the acrylic ester high molecular type monomer that diallyl glycol ether two carbonate monomers that methyl methacrylate, vinylbenzene, refractive index are 1.49, the acrylic ester high molecular type monomer that refractive index is 1.56 and refractive index are 1.60.
Anti-blue light nano-composite resin material as above, preferably, the particle diameter of described hud typed transition metal oxide nano-particles is 20-50nm; Its kernel is transition metal oxide, and this transition metal oxide is TiO
2, CoO and Fe
2o
3in at least one, while using more than one transition metal oxides, mix according to arbitrary proportion; Shell is tensio-active agent, and thickness is 3-10nm.
Anti-blue light nano-composite resin material as above, preferably, described tensio-active agent is C
2-C
5carboxylate salt, Polyvinylpyrolidone (PVP) or Sodium dodecylbenzene sulfonate.
Anti-blue light nano-composite resin material as above, preferably, described UV light absorber is fat-soluble UV light absorber.
Anti-blue light nano-composite resin material as above, preferably, described fat-soluble UV light absorber is at least one in UV-P, UV-326, UV-327, UV-328, UV-329, UV-360, UV-531 and UV-928, while using multiple UV light absorber, mixes according to arbitrary proportion.
Anti-blue light nano-composite resin material as above, preferably, the preparation method of described hud typed transition metal oxide nano-particles is as follows:
In the transition metal salt solution that is 0.1～1mol/L to concentration, drip H
2sO
4the aqueous solution to solution is transparence, then dripping alkaline aqueous solution makes to settle out, aqueous solution pH is between 7-12, at 50 DEG C, acid adding makes resolution of precipitate, obtains the transition metal oxide water-sol, and pH is between 1-7, add tensio-active agent and/or ammoniacal liquor or sodium acetate as consisting of phase-transferring agent, the triangular molar ratio scope of transition metal salt, tensio-active agent and consisting of phase-transferring agent is 1: (0.1-10): (0-1); Stir 1-120 minute, forming transition metal oxide cluster is core, the nano particle taking coating materials as shell; Through the transition metal oxide nano particle that dewaters, dries loosely.
On the other hand, the invention provides the preparation method of anti-blue light nano-composite resin material as above, the method comprises the steps:
A. prepolymerization: add initiator in the nano combined monomer material of described anti-blue light, prepolymerization is carried out in heating, obtains prepolymer;
B. after polymerization: the temperature programming of carrying out after the μ m filter screen/membrane filtration of above-mentioned prepolymer via hole diameter≤1 10-20 hour is solidified, and solidification value rises to 85 DEG C from room temperature; Then at 100-160 DEG C of curing 2-6 hour, obtain anti-blue light optical resin material.
For thermoplastic resin material, prepare anti-blue light nano-composite resin material and also can adopt following methods:
Method 1:
A. thermoplasticity optical resin is dissolved in solvent, obtains optical resin solution;
B. take hud typed transition metal oxide nano-particles and UV light absorber by said ratio, and join in above-mentioned resin solution, after stirring and dissolving is even, spin coating obtains the nano combined optical resin material of anti-blue light.
Method 2:
A. take thermoplasticity optical resin powder, hud typed transition metal oxide nano-particles and UV light absorber by said ratio, high-speed stirring mixes;
B. said mixture melt blending is made to the nano combined optical resin material of anti-blue light.
On the one hand, the invention provides a kind of anti-blue light nanocomposite eyeglass again, this resin lens adopts anti-blue light nano-composite resin material as above to make.
Anti-blue light nanocomposite eyeglass as above, preferably, in this eyeglass, described hud typed transition metal oxide nano-particles accounts for the 0.5%-2% of described total resin weight, and described UV light absorber accounts for the 1%-3% of described total resin weight.
Nanocomposite eyeglass as above, preferably, the center thickness of described resin lens is 1.0-2.0mm.
Another aspect, the invention provides the preparation method of eyeglass described above, and the method comprises the steps:
A. take for the preparation of the high polymer monomer of described macromolecule resin, hud typed transition metal oxide nano-particles and UV light absorber by proportioning described above; Hud typed transition metal oxide nano-particles joins in high polymer monomer, and magnetic agitation is dispersed in high polymer monomer nanoparticle, and via hole diameter≤0.45 μ m filter paper/membrane filtration is for subsequent use;
B. prepolymerization: add UV light absorber in the mixed solution obtaining to steps A, stir after UV light absorber is dissolved completely and add initiator, prepolymerization is carried out in heating, obtains prepolymer;
C. mold filling solidifies: will after the μ m filter paper/membrane filtration of above-mentioned prepolymer via hole diameter≤1, insert in mould cavity, put it into subsequently the temperature programming of carrying out 15-20 hour in temperature programming stove and solidify, solidification value rises to 85 DEG C from room temperature; Be cooled to die sinking after room temperature, edging, cleaning;
D. regelate: eyeglass clean above-mentioned edging is put into regelate stove, at 120-140 DEG C of curing 2-3 hour, obtain optical resin lens.
Method as above, preferably, in the prepolymerization of described step B,
When high polymer monomer is diallyl glycol ether two carbonate monomer of refractive index 1.49, prepolymerization carries out at 45-50 DEG C, initiator is di-isopropyl peroxydicarbonate, and initiator add-on is the 2.5-2.8% of high polymer monomer weight, and the prepolymerization time is 2-5 hour;
When high polymer monomer is the acrylic ester high molecular type monomer of refractive index 1.56, prepolymerization carries out at 45-50 DEG C, initiator is di-isopropyl peroxydicarbonate, and initiator add-on is the 2.5-2.8% of high polymer monomer weight, and the prepolymerization time is 2-5 hour;
When high polymer monomer is the acrylic ester high molecular type monomer of refractive index 1.60, prepolymerization carries out at 70-80 DEG C, and initiator is azo-bis-isobutyl cyanide, and initiator add-on is the 0.5-1.0% of high polymer monomer weight, and the prepolymerization time is 2-5 hour.
Another aspect, the invention provides a kind of anti-blue light nanocomposite eyeglass, and it is that application method described above is manufactured.
Another aspect, the invention provides nano-composite resin material described above in the application of preparing the optical protective material fields such as blue light protection glass, LED display protective film, LED lamp protective film, automobile lamp, optical protection glass.
Hud typed transition metal oxide nano particle used in the present invention can be bought in market, the hud typed transition metal oxide nano particle that for example Jiangsu Huatiantong Technology Co., Ltd. produces, also can for example, according to known method preparation, disclosed method in patent No. ZL96101878.X.Preferably, adopt and prepare with the following method hud typed transition metal oxide nano-particles:
In the transition metal salt solution that is 0.1～1mol/L to concentration, drip H
2sO
4the aqueous solution to solution is transparence, then dripping alkaline aqueous solution makes to settle out, aqueous solution pH is between 7-12, at 50 DEG C, acid adding makes resolution of precipitate, obtains the transition metal oxide water-sol, and pH is between 1-7, add tensio-active agent and/or ammoniacal liquor or sodium acetate as consisting of phase-transferring agent, the triangular molar ratio scope of transition metal salt, tensio-active agent and consisting of phase-transferring agent is 1: (0.1-10): (0-1); Stir 1-120 minute, forming transition metal oxide cluster is core, the nano particle taking coating materials as shell; Through the transition metal oxide nano particle that dewaters, dries loosely.
Beneficial effect of the present invention is: the hud typed transition metal oxide that adulterated in resin lens of the present invention (titanium dioxide, cobalt oxide and/or ferric oxide) nano particle and UV light absorber, by simple and effective manufacturing process, just can prepare over-all properties comprehensively and excellent high-performance anti-blue light resin lens.Nano particle and UV light absorber are brought into play to act synergistically and are given the anti-blue light performance of this nanocomposite eyeglass excellence in resin matrix, can shield high energy blue light and the ultraviolet ray of wavelength at the harm human eye of 380-450nm scope by high-efficient and lasting.In addition, nano-grade size and nucleocapsid structure make nano particle and macromolecule resin base material have splendid interfacial phase dissolubility, therefore its in resin base material, be uniformly dispersed, good stability, give eyeglass all can be clear under strong and weak luminous environment depending on thing and distinguish the excellent optical property that look soft.
Brief description of the drawings
Fig. 1 is 1.60 refractive index resin eyeglass anti-blue light effect comparison spectrograms.
Fig. 2 is different content TiO prepared by embodiment 1
2anti-blue light PMMA/TiO
2resin sheet spectrogram.
Fig. 3 is different content TiO prepared by embodiment 2
2anti-blue light PMS/TiO
2resin sheet spectrogram.
Fig. 4 is 1.49 specific refractory power different content TiO prepared by embodiment 5
2anti-blue light resin lens spectrogram.
Fig. 5 is 1.56 specific refractory power different content TiO prepared by embodiment 6
2anti-blue light resin lens spectrogram.
Fig. 6 is 1.60 specific refractory power different content TiO prepared by embodiment 7
2anti-blue light resin lens spectrogram.
Embodiment
Principle of design of the present invention is as follows:
(1) determine protection wavelength region
Medical research shows, the purple light of human eye to 380-450nm wave band and part blue light depending on thing and distinguish that look insensitive, and this band of light wave-wave length energy is high, large to eye injury.Consider ultraviolet ray, determine and need suitably the shielding following blue light of 450nm and ultraviolet ray, the above part blue light of 450nm and visible ray are kept to rational transmitance.
Table 1: anti-blue light resin sheet blue light protection wavelength region
| Wavelength region (nm) | Represent wavelength (nm) |
| 380-430 | 405 |
| 430-450 | 440 |
| 450-500 | 475 |
(2) design anti-blue light resin material transmitance scope
According to the blue light protection wavelength region of formulating, make anti-blue light resin material reach following table at the peak transmittance at the representative wavelength place of ultraviolet and visible region and require:
Table 2 anti-blue light resin resin material design transmitance
(3) determine composition, proportioning and the preparation condition of transition metal oxide nano-particles and UV light absorber in anti-blue light resin material.
Existing research shows, compared with virgin resin base material, at 360-450nm has stronger absorption effects after mixing transition metal oxide nano-particles in resin base material, and the extinction scope of mixing the resin base material of UV light absorber is generally 360-410nm.Investigator of the present invention surprisingly finds, in the time that the transition metal oxide nano-particles of suitable proportion and UV light absorber are scattered in resin base material jointly, its absorbing wavelength is compared the wavelength generation red shift of mixing separately transition metal oxide nano-particles or UV light absorber, as shown in Figure 1, it is that thickness is 2mm, 1.60 refractive index resin sheet material anti-blue light effect comparison spectrograms.The present invention utilizes this synergy, according to the anti-blue light eyeglass transmitance scope of above formulation, to one or more transition metal oxide nano-particles and UV light absorber carry out composite and and resin compounded, prepare can high-efficiency shielding 380-450nm scope blue light and all ultraviolet rays, all can be clear under strong and weak luminous environment depending on thing, distinguish high-performance anti-blue light resin material and the eyeglass of and the wear-resisting and Good Heat-resistance of look soft.Research shows, the resin material that is 0.1-10mm for thickness, when one or more nanoparticle total amounts account for the 0.2%-2% of resin lens material gross weight, when the total amount of one or more UV light absorber accounts for the 0.5%-5% of resin lens material gross weight, can realize the transmitance scope of design of above-mentioned blue light protection wavelength region may.
Below by specific embodiment, the invention will be further described, but and do not mean that limiting the scope of the invention.
The hud typed transition metal oxide using in following examples is Jiangsu Huatiantong Technology Co., Ltd. and produces.The particle diameter of this hud typed transition metal oxide nano-particles is 20-50nm; Its kernel is TiO
2, CoO or Fe
2o
3; Shell is sodium acetate tensio-active agent, and thickness is 3-10nm.
Embodiment 1 prepares anti-blue light PMMA/TiO
2compound resin sheet material
Taking 2.0g titanium dioxide nano-particle joins in 100g methyl methacrylate monomer, magnetic agitation, after being uniformly dispersed through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-328 and UV-329), after being uniformly mixed, add initiator dibenzoyl peroxide 1.0g, stirring at low speed under 200r/min, be controlled at 80 DEG C polyreaction 3 hours, complete prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, and the thickness of mould is 3mm, in curing oven, rises to 85 DEG C through 20 hours from room temperature, completes one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 120 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin sheet of nano-titania particle.
By above-mentioned same method, preparation different Ti O2 content anti-blue light resin sheet, replaces 2.0g titanium dioxide nano-particle with 0g titanium dioxide nano-particle in step, and accurate solidification value replaces 120 DEG C by 105 DEG C.
Fig. 2 is equivalent ultraviolet radiation absorption agent content (2%) different Ti O
2the anti-blue light PMMA/TiO of content
2the ultraviolet-visible spectrogram of resin sheet.As we know from the figure: core-shell type nano TiO
2give the anti-blue light performance of compound resin sheet material excellence with the synergy of UV light absorber, and in the situation that ultraviolet radiation absorption dosage is fixing, increase nano-TiO
2content, resin sheet increases in the absorption spectrum Einstein shift amount in ultraviolet-visible district, blue light absorption ability strengthens.Resin sheet is greater than 83% to the above visible light transmissivity of 500nm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 2 prepares anti-blue light PMS/TiO
2compound resin sheet material
Taking 2.0g titanium dioxide nano-particle joins in 10g methyl methacrylate and the cinnamic mix monomer of 90g, magnetic agitation, after being uniformly dispersed through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 1.0g, stirring at low speed under 200r/min, be controlled at 80 DEG C polyreaction 3 hours, complete prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, and the thickness of mould is 3mm, in curing oven, rises to 85 DEG C through 20 hours from room temperature, completes one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 120 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin sheet of nano-titania particle.
By above-mentioned same method, preparation different Ti O
2content anti-blue light resin sheet, replaces 2.0g titanium dioxide nano-particle with 0g titanium dioxide nano-particle in step, and accurate solidification value replaces 120 DEG C by 100 DEG C.
Fig. 3 is equivalent ultraviolet radiation absorption agent content (2%) different Ti O
2the anti-blue light PMS/TiO of content
2the ultraviolet-visible spectrogram of resin sheet.As we know from the figure: core-shell type nano TiO
2give the anti-blue light performance of compound resin sheet material excellence with the synergy of UV light absorber, and in the situation that ultraviolet radiation absorption dosage is fixing, increase nano-TiO
2content, resin sheet increases in the absorption spectrum Einstein shift amount in ultraviolet-visible district, blue light absorption ability strengthens.Resin sheet is greater than 81% to the above visible light transmissivity of 500nm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 3 prepares anti-blue light PMS/TiO
2compound resin sheet material
Taking 2.0g titanium dioxide nano-particle joins in 50g methyl methacrylate and the cinnamic mix monomer of 50g, magnetic agitation, after being uniformly dispersed through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 1.0g, stirring at low speed under 200r/min, be controlled at 80 DEG C polyreaction 3 hours, complete prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, and the thickness of mould is 3mm, in curing oven, rises to 85 DEG C through 20 hours from room temperature, completes one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 120 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin sheet of nano-titania particle.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 4 prepares anti-blue light PMS/TiO
2compound resin sheet material
Taking 2.0g titanium dioxide nano-particle joins in 90g methyl methacrylate and the cinnamic mix monomer of 10g, magnetic agitation, after being uniformly dispersed through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 1.0g, stirring at low speed under 200r/min, be controlled at 80 DEG C polyreaction 3 hours, complete prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, and the thickness of mould is 3mm, in curing oven, rises to 85 DEG C through 20 hours from room temperature, completes one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 120 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin sheet of nano-titania particle.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 5 prepares 1.49 specific refractory power anti-blue light TiO
2compound resin eyeglass
Taking the hud typed titanium dioxide nano-particle of 0.5g, to join 100g specific refractory power be in 1.49 diallyl glycol ether two carbonate monomers, magnetic agitation, after being uniformly dispersed through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-328 and UV-329), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, be controlled at 45 DEG C polyreaction 3 hours, complete prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin lens of nano-titania particle, and center thickness is 2mm.
By above-mentioned same method, preparation different Ti O
2content anti-blue light resin lens, replaces 0.5g titanium dioxide nano-particle with 0g titanium dioxide nano-particle, 1.0g titanium dioxide nano-particle, 2.0g titanium dioxide nano-particle in step.
Fig. 4 is equivalent ultraviolet radiation absorption agent content (2%) different Ti O
2the ultraviolet-visible spectrogram of 1.49 specific refractory power anti-blue light resin lens of content.As we know from the figure: core-shell type nano TiO
2give the anti-blue light performance of resin lens excellence with the synergy of UV light absorber, and in the situation that ultraviolet radiation absorption dosage is fixing, along with the increase of nanometer content, eyeglass increases in the absorption spectrum Einstein shift amount in ultraviolet-visible district, and blue light absorption ability strengthens.Eyeglass is greater than 84% to the above visible light transmissivity of 500nm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 6 prepares 1.56 specific refractory power anti-blue light TiO
2compound resin eyeglass
Taking the hud typed titanium dioxide nano-particle of 0.5g, to join 100g specific refractory power be in 1.56 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-360 and UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, is controlled at 50 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2.5 hours, completes regelate, must be containing the anti-blue light resin lens of titanium dioxide nano-particle, and center thickness is 2mm.
By above-mentioned same method, preparation different Ti O
2content anti-blue light resin lens, replaces 0.5g titanium dioxide nano-particle with 0g titanium dioxide nano-particle, 1.0g titanium dioxide nano-particle, 2.0g titanium dioxide nano-particle in step.
Fig. 5 is equivalent ultraviolet radiation absorption agent content (2%) different Ti O
2the ultraviolet-visible spectrogram of 1.56 specific refractory power anti-blue light resin lens of content.As we know from the figure: core-shell type nano TiO
2give with the synergy of UV light absorber the anti-blue light performance that resin lens is good, and in the situation that ultraviolet radiation absorption dosage is fixing, along with the increase of nanometer content, eyeglass increases in the absorption spectrum Einstein shift amount in ultraviolet-visible district, and blue light absorption ability strengthens.Eyeglass is greater than 84% to the above visible light transmissivity of 500nm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 7 prepares 1.60 specific refractory power anti-blue light TiO
2compound resin eyeglass
Taking the hud typed titanium dioxide nano-particle of 0.5g, to join 100g specific refractory power be in 1.60 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 0.8g, 200r/min stirring at low speed, is controlled at 75 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 3 hours, completes regelate, must be containing the anti-blue light resin lens of titanium dioxide nano-particle, and center thickness is 2mm.
By above-mentioned same method, preparation different Ti O
2content anti-blue light resin lens, replaces 0.5g titanium dioxide nano-particle with 0g titanium dioxide nano-particle, 1.0g titanium dioxide nano-particle, 2.0g titanium dioxide nano-particle in step.
Fig. 6 is equivalent ultraviolet radiation absorption agent content (2%) different Ti O
2the ultraviolet-visible spectrogram of 1.60 specific refractory power anti-blue light resin lens of content.As we know from the figure: core-shell type nano TiO
2give with the synergy of UV light absorber the anti-blue light performance that resin lens is good, and in the situation that ultraviolet radiation absorption dosage is fixing, along with the increase of nanometer content, eyeglass increases in the absorption spectrum Einstein shift amount in ultraviolet-visible district, and blue light absorption ability strengthens.Eyeglass is greater than 80% to the above visible light transmissivity of 500nm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 8 prepares 1.49 specific refractory power anti-blue light CoO compound resin eyeglasses
Taking the hud typed cobalt oxide nanoparticle of 0.5g, to join 100g specific refractory power be in 1.49 diallyl glycol ether two carbonate monomers, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 3.0g UV light absorber (the each 1.5g of UV-328 and UV-329), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, is controlled at 45 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin lens of cobalt oxide nanoparticle, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 9 prepares 1.56 specific refractory power anti-blue light CoO compound resin eyeglasses
Taking the hud typed cobalt oxide nanoparticle of 1.0g, to join 100g specific refractory power be in 1.56 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 3.0g UV light absorber (the each 1.5g of UV-360 and UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.6g, stirring at low speed, is controlled at 50 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2.5 hours, completes regelate, must be containing the anti-blue light resin lens of cobalt oxide nanoparticle, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 10 prepares 1.60 specific refractory power anti-blue light CoO compound resin eyeglasses
Taking the hud typed cobalt oxide nanoparticle of 2.0g, to join 100g specific refractory power be in 1.60 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 3.0g UV light absorber (the each 1.5g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 0.8g, stirring at low speed under 200r/min, is controlled at 75 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 3 hours, completes regelate, must be containing the anti-blue light resin lens of cobalt oxide nanoparticle, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 11 prepares 1.49 specific refractory power anti-blue light Fe
2o
3compound resin eyeglass
Taking the hud typed ferric oxide nano particles of 0.5g, to join 100g specific refractory power be in 1.49 diallyl glycol ether two carbonate monomers, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-360 and UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, is controlled at 45 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin lens of ferric oxide nano particles, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 12 prepares 1.56 specific refractory power anti-blue light Fe
2o
3compound resin eyeglass
Taking the hud typed ferric oxide nano particles of 1.0g, to join 100g specific refractory power be in 1.56 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 2.0g UV light absorber (the each 1.0g of UV-360 and UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.8g, 200r/min stirring at low speed, is controlled at 50 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 3 hours, completes regelate, must be containing the anti-blue light resin lens of ferric oxide nano particles, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 13 prepares 1.60 specific refractory power anti-blue light Fe
2o
3compound resin eyeglass
Taking the hud typed ferric oxide nano particles of 1.5g, to join 100g specific refractory power be in 1.60 acrylate monomer, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 3.0g UV light absorber (the each 1.5g of UV-326 and UV-327), after being uniformly mixed, add initiator Diisopropyl azodicarboxylate 0.8g, 200r/min stirring at low speed, is controlled at 75 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 3 hours, completes regelate, must be containing the anti-blue light resin lens of ferric oxide nano particles, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 14 prepares 1.49 specific refractory power anti-blue light nanocomposite eyeglasses
Taking 0.2g titanium dioxide, 0.2g cobalt oxide, 0.1g ferric oxide nano particles, to join 100g specific refractory power be in 1.49 diallyl glycol ether two carbonate monomers, magnetic agitation and be uniformly dispersed after through 0.45 μ m filter paper filtering, add 3.0g UV light absorber (the each 1.5g of UV-360 and UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, is controlled at 45 DEG C polyreaction 3 hours, completes prepolymerization; Pre-polymerization mixture is injected to mould through 1 μ m strainer filtering, after degassed, in curing oven, rose to 85 DEG C through 20 hours from room temperature, complete one-step solidification; One-step solidification finishes, and die sinking is cleaned, and in accurate curing oven, 140 DEG C of constant temperature 2 hours, completes regelate, must be containing the anti-blue light resin lens of composite nanoparticle, and center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and UV spectrum district transmittance the results are shown in Table 4.
Embodiment 15: anti-blue light resin lens transmitance test experience
Resin lens UV, visible light light transmission rate prepared by embodiment 1-10 detects and selects the Shanghai UV-8000 of Yuan Xi Instrument Ltd. type ultraviolet-visible photometer, and result is as shown in table 3, table 4.From table, result is learnt: the anti-blue light eyeglass of manufacture of the present invention can effectively shield most of high energy blue light below 450nm and all ultraviolet rays, to visible light transmissivity more than 500nm higher than 80%.Eyeglass has excellent clear thing, the soft performance of variable color of looking under strong and weak luminous environment in effective anti-blue light, and detected result is listed in the table below.
Table 3 anti-blue light resin lens visible region transmitance Eurya plant is surveyed result
Table 4 anti-blue light resin lens UV spectrum district transmittance detected result
Claims (10)
1. an anti-blue light nano-composite resin material, is characterized in that, this material comprises the macromolecule resin for making optical material and is scattered in hud typed transition metal oxide nano-particles and the UV light absorber of macromolecule resin; Wherein, hud typed transition metal oxide nano-particles accounts for the 0.2%-2% of total resin weight, and UV light absorber accounts for the 0.5%-5% of total resin weight.
2. anti-blue light nano-composite resin material as claimed in claim 1, it is characterized in that, described is to be polymerized by high polymer monomer for making the macromolecule resin of optical material, and this high polymer monomer is selected from: at least one in vinyl monomer, acrylate type monomer, allyl type monomer, epoxy resin high polymer monomer, polycarbonate-based high polymer monomer and polyurethane series high polymer monomer.
3. anti-blue light nano-composite resin material as claimed in claim 2, it is characterized in that, described high polymer monomer is selected from: at least one in the acrylic ester high molecular type monomer that diallyl glycol ether two carbonate monomers that methyl methacrylate, vinylbenzene, refractive index are 1.49, the acrylic ester high molecular type monomer that refractive index is 1.56 and refractive index are 1.60.
4. anti-blue light nano-composite resin material as claimed in claim 1, is characterized in that, the particle diameter of described hud typed transition metal oxide nano-particles is 20-50nm; Its kernel is transition metal oxide, and this transition metal oxide is TiO
2, CoO and Fe
2o
3in at least one, while using more than one transition metal oxides, mix according to arbitrary proportion; Shell is tensio-active agent, and thickness is 3-10nm; Described tensio-active agent is C
2-C
5carboxylate salt, Polyvinylpyrolidone (PVP) or Sodium dodecylbenzene sulfonate.
5. anti-blue light nano-composite resin material as claimed in claim 1, it is characterized in that, described UV light absorber is fat-soluble UV light absorber, this fat-soluble UV light absorber is at least one in UV-P, UV-326, UV-327, UV-328, UV-329, UV-360, UV-531 and UV-928, while using multiple UV light absorber, mixes according to arbitrary proportion.
6. the preparation method of the anti-blue light nano-composite resin material as described in any one in claim 1-5, is characterized in that, the method comprises the steps:
A. prepolymerization: add initiator in the nano combined monomer material of described anti-blue light, prepolymerization is carried out in heating, obtains prepolymer;
B. after polymerization: the temperature programming of carrying out after the μ m filter screen/membrane filtration of above-mentioned prepolymer via hole diameter≤1 10-20 hour is solidified, and solidification value rises to 85 DEG C from room temperature; Then at 100-160 DEG C of curing 2-6 hour, obtain anti-blue light optical resin material.
7. an anti-blue light nanocomposite eyeglass, is characterized in that, this resin lens is to adopt the anti-blue light nano-composite resin material described in any one in claim 1-5 to make.
8. anti-blue light nanocomposite eyeglass as claimed in claim 7, it is characterized in that, in this eyeglass, described hud typed transition metal oxide nano-particles accounts for the 0.5%-2% of described total resin weight, and described UV light absorber accounts for the 1%-3% of described total resin weight.
9. the preparation method of anti-blue light nanocomposite eyeglass as claimed in claim 7 or 8, is characterized in that, the method comprises the steps:
A. take for the preparation of the high polymer monomer of described macromolecule resin, hud typed transition metal oxide nano-particles and UV light absorber by proportioning described in claim 1; Hud typed transition metal oxide nano-particles joins in high polymer monomer, and magnetic agitation is dispersed in high polymer monomer nanoparticle, and via hole diameter≤0.45 μ m filter paper/membrane filtration is for subsequent use;
B. prepolymerization: add UV light absorber in the mixed solution obtaining to steps A, stir after UV light absorber is dissolved completely and add initiator, prepolymerization is carried out in heating, obtains prepolymer;
C. mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after the μ m filter paper/membrane filtration of via hole diameter≤1, put it into subsequently the temperature programming of carrying out 15-20 hour in temperature programming stove and solidify, solidification value rises to 85 DEG C from room temperature; Be cooled to die sinking after room temperature, edging, cleaning;
D. regelate: eyeglass clean above-mentioned edging is put into regelate stove, at 120-140 DEG C of curing 2-3 hour, obtain optical resin lens.
10. method as claimed in claim 9, is characterized in that, in the prepolymerization of described step B,
When high polymer monomer is diallyl glycol ether two carbonate monomer of refractive index 1.49, prepolymerization carries out at 45-50 DEG C, initiator is di-isopropyl peroxydicarbonate, and initiator add-on is the 2.5-2.8% of high polymer monomer weight, and the prepolymerization time is 2-5 hour;
When high polymer monomer is the acrylic ester high molecular type monomer of refractive index 1.56, prepolymerization carries out at 45-50 DEG C, initiator is di-isopropyl peroxydicarbonate, and initiator add-on is the 2.5-2.8% of high polymer monomer weight, and the prepolymerization time is 2-5 hour;
When high polymer monomer is the acrylic ester high molecular type monomer of refractive index 1.60, prepolymerization carries out at 70-80 DEG C, and initiator is azo-bis-isobutyl cyanide, and initiator add-on is the 0.5-1.0% of high polymer monomer weight, and the prepolymerization time is 2-5 hour.
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