CN103980643B - Anti-blue light nano-composite resin material, eyeglass and preparation method thereof - Google Patents
Anti-blue light nano-composite resin material, eyeglass and preparation method thereof Download PDFInfo
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Abstract
A kind of anti-blue light nano-composite resin material, eyeglass and its manufacture method, the material include the hud typed transition metal oxide nano-particles and ultra-violet absorber for making the macromolecule resin of optical material and being scattered in macromolecule resin；Wherein, hud typed transition metal oxide nano-particles account for 0.2% the 2% of total resin weight, and ultra-violet absorber accounts for 0.5% the 5% of total resin weight.The particle diameter of nano-particle is 20 50nm；Shell is surfactant, and thickness is 3 10nm.Nano-particle is well-dispersed in high polymer monomer with ultra-violet absorber, through prepolymerization --- the technical process of after polymerization, anti-blue light composite resin material is obtained.Present invention process is simple, favorable reproducibility, the high energy harmful blue light and ultraviolet of obtained resin material and eyeglass energy high-efficient and lasting shielding wavelength in the range of 380 450nm, clearly depending on thing and can distinguish that color is soft under strong and weak luminous environment, with excellent combination property.
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 nanocomposite
Material, eyeglass and preparation method thereof.
Background technology
It is well known that ultraviolet has strong detrimental effect to eyes.Eyes under ultraviolet, easily draw for a long time
From cataract or glaucoma, cause retinal pigment epithelium to damage, cause and even accelerate age related macular degeneration etc..Additionally, there is research table
It is bright, it is seen that the blue light (wavelength is the short wavelength light of 380-500nm scopes) in light can penetrate crystalline lens and reach retina, retina
Free radical can be produced through blue light long-term irradiation, and these free radicals can cause retinal pigment epithelium to become feeble and die, and then cause
Photosensitive cell lacks nutrient, finally causes vision impairment.And its extent of damage increases sharply with the reduction of optical wavelength.It is blue
Light is studied confirms it is the visible ray for most endangering.Medical research is also shown that purple light and part of the human eye to 380-450nm wave bands
Blue light depending on thing and distinguishing that color is insensitive, i.e. eyes are limited to the color discrimination ability of the coloured light of the wave band, but the wave band light wave ripple
Length energy is high, larger to eye injury.Therefore, below 450nm blue lights and ultraviolet irradiation are prevented effectively to protect eyes
It is most important.
With the progress and development of modern society, LED, TV, computer display screen, smart mobile phone, panel computer etc. are produced
Product have been widely used in the every aspect of people's life, in the light that these products (especially LED and display screen) send
High energy shortwave blue light containing a large amount of irregular frequencies.Image, word, video etc. are closely watched for a long time, eyes can be made
Into certain pressure, and then there is blood-shot eye illness, eye is done, and eye is puckery, eye-blurred, asthenopia, head, back, shoulder and cervical vertebra ache etc.
Symptom.Therefore, for worker for a long time indoors under outer strong light environment, have patient, student race from cataract or glaucoma and ARM
And for the working clan of long-term use computer, it is very necessary and the most simple and effective method to wear anti-blue light glasses.
Present many anti-blue light resin lens are that doping or surface dip-dye melanin, uranidin etc. are organic in lens substrate
Coloring agent, certain blue light neutralization, filter effect is reached using the neutralization principle of optical color.But, because organic dyestuff is resistance to
Time property is weaker, can be faded through sunlight long-term irradiation, it is impossible to durable in use.Additionally, the blue light percent of pass of many eyeglasses is less than 10%,
Thus again by the further absorption of crystalline lens in eyes and vitreum, real arrival human eye after this anti-blue light glasses high is worn
The blue light amount of retina is almost nil, that is, intercepts the blue coloured light in coloured light three primary colours (red, green, blue) completely, as a result can
Picture serious distortion is caused, the color sense lightsensitivity of optic nerve can be if things go on like this reduced, there is the wind for causing anomalous trichromatism or even colour blindness
Danger.Moreover, coloured anti-blue light eyeglass is relatively low to the selective transmitance of long wave visible ray, and thing and chromatic discrimination power are regarded when wearing
Weaker, especially under cloudy day or low light environment, the uniform validity improved method taken at this stage is to be deposited with 3-11 layers even more
The anti-reflection film of multilayer, manufacturing process is numerous and diverse and antireflective effect is limited.Therefore, simple and effective manufacturing process is sought, and then is manufactured
Go out high-performance anti-blue light resin material, the eyeglass of excellent combination property, high-efficient and lasting anti-blue light is made it have, under strong and weak luminous environment
Clearly depending on thing and the soft excellent properties of color can be distinguished, it is significant.
The content of the invention
The present invention is in view of the shortcomings of the prior art, there is provided a kind of anti-blue light nano-composite resin material, eyeglass and its system
Method is made, the manufacturing approach craft is simple, favorable reproducibility, is greatly improved industrial production efficiency；Obtained resin material, mirror
Piece energy high-efficient and lasting shields high energy harmful blue light and ultraviolet of the wavelength in 380-450nm scopes, can be clear under strong and weak luminous environment
Clear depending on thing and to distinguish that color is soft, combination property is good.
To achieve the above object, the present invention includes following technical scheme：
A kind of anti-blue light nano-composite resin material, the material include for make optical material macromolecule resin and
It is scattered in hud typed transition metal oxide nano-particles and ultra-violet absorber in macromolecule resin；Wherein, hud typed mistake
The 0.2%-2% that metal oxide nanoparticles account for total resin weight is crossed, ultra-violet absorber accounts for the 0.5%- of total resin weight
5%.
Anti-blue light nano-composite resin material as described above, it is preferable that the macromolecule for making optical material
Resin is polymerized by high polymer monomer, and the high polymer monomer is selected from：Vinyl monomer, acrylate-type monomer, pi-allyl
In type monomer, epoxy resin high polymer monomer, polycarbonate-based high polymer monomer and polyurethane series high polymer monomer at least
It is a kind of.It is highly preferred that the high polymer monomer is selected from：Methyl methacrylate, styrene, refraction index are 1.49 diallyl
Diethylene glycol biscarbonate monomer, refraction index are 1.56 acrylic ester high molecular type monomer and propylene that refraction index is 1.60
At least one in esters of gallic acid high polymer monomer.
Anti-blue light nano-composite resin material as described above, it is preferable that the hud typed transition metal oxide nano
The particle diameter of particle is 20-50nm；Its kernel is transition metal oxide, and the transition metal oxide is TiO2, CoO and Fe2O3In
At least one, during using more than one transition metal oxides according to arbitrary proportion mix；Shell is surfactant, thickness
It is 3-10nm.
Anti-blue light nano-composite resin material as described above, it is preferable that the surfactant is C2-C5It is carboxylate, poly-
Vinyl pyrrolidone or neopelex.
Anti-blue light nano-composite resin material as described above, it is preferable that the ultra-violet absorber is fat-soluble ultraviolet
Light absorbers.
Anti-blue light nano-composite resin material as described above, it is preferable that the fat-soluble ultra-violet absorber be UV-P,
At least one in UV-326, UV-327, UV-328, UV-329, UV-360, UV-531 and UV-928, uses various ultraviolets
Mix according to arbitrary proportion during absorbent.
Anti-blue light nano-composite resin material as described above, it is preferable that the hud typed transition metal oxide nano
The preparation method of particle is as follows：
H is added dropwise in the transition metal salt solution for concentration being 0.1~1mol/L2SO4The aqueous solution to the transparent shape of solution, so
Alkaline aqueous solution is added dropwise afterwards makes precipitation settle out, and between 7-12, at 50 DEG C, acid adding dissolves precipitation to aqueous solution pH, obtains transition
The metal oxide hydrosol, pH adds surfactant and/or the ammoniacal liquor or sodium acetate as consisting of phase-transferring agent, transition between 1-7
Slaine, surfactant and the triangular molar ratio of consisting of phase-transferring agent are 1: (0.1-10): (0-1)；1-120 points of stirring
Clock, forms transition metal oxide cluster for core, the nano particle with coating material as shell；Through be dehydrated, dry loosely
Transition metal oxide nano particle.
On the other hand, the present invention provides the preparation method of anti-blue light nano-composite resin material as described above, the method
Comprise the following steps：
A. prepolymerization：To initiator is added in the nano combined monomer material of the anti-blue light, heating carries out prepolymerization,
Obtain prepolymer；
B. after polymerization：The program of 10-20 hours will be carried out after above-mentioned prepolymer via hole diameter≤1 μm filter screen/membrane filtration
Elevated cure, solidification temperature rises to 85 DEG C from room temperature；Then solidify 2-6 hours at 100-160 DEG C, obtain anti-blue light optical resin
Material.
For thermoplastic resin material, preparing anti-blue light nano-composite resin material can also use following methods：
Method 1：
A. plastic optical resin is dissolved in solvent, obtains optical resin solution；
B. hud typed transition metal oxide nano-particles and ultra-violet absorber are weighed by said ratio, and is added to
State in resin solution, after stirring and dissolving is uniform, spin coating obtains the nano combined optics resin material of anti-blue light.
Method 2：
A. plastic optical resin's powder, hud typed transition metal oxide nano-particles and ultraviolet are weighed by said ratio
Light absorbers, high-speed stirred is well mixed；
B. said mixture melt blending is obtained the nano combined optics resin material of anti-blue light.
Another further aspect, the present invention provides a kind of anti-blue light nanocomposite eyeglass, and the resin lens are using as above institute
What the anti-blue light nano-composite resin material stated was made.
Anti-blue light nanocomposite eyeglass as described above, it is preferable that in the eyeglass, the hud typed oxo transition metal
Compound nano-particle accounts for the 0.5%-2% of the total resin weight, and the ultra-violet absorber accounts for the total resin weight
1%-3%.
Nanocomposite eyeglass as described above, it is preferable that the center thickness of the resin lens is 1.0-2.0mm.
Another aspect, the present invention provides the preparation method of eyeglass as described above, and the method comprises the following steps：
A. proportioning weighs high polymer monomer, the hud typed transition metal for preparing the macromolecule resin as described above
Oxide nano-particles and ultra-violet absorber；Hud typed transition metal oxide nano-particles are added in high polymer monomer,
Magnetic agitation makes nano-particle be dispersed in high polymer monomer, and via hole diameter≤0.45 μm filter paper/membrane filtration is standby；
B. prepolymerization：To ultra-violet absorber is added in the mixed liquor that step A is obtained, stirring ultra-violet absorber is completely molten
Initiator is added after solution, heating carries out prepolymerization, obtains prepolymer；
C. mold filling solidification：In inserting mould cavity after above-mentioned prepolymer via hole diameter≤1 μm filter paper/membrane filtration, then
The temperature programming that put it into is carried out 15-20 hours in temperature programming stove solidifies, and solidification temperature rises to 85 DEG C from room temperature；It is cooled to
Die sinking, edging, cleaning after room temperature；
D. two solidifications：The eyeglass that above-mentioned edging is cleaned is put into secondary curing oven, it is small to solidify 2-3 at 120-140 DEG C
When, obtain optical resin lens.
Method as described above, it is preferable that in the prepolymerization of the step B,
When high polymer monomer is the diallyl diethylene glycol biscarbonate monomer of refraction index 1.49, prepolymerization exists
45-50 DEG C is carried out, and initiator is di-isopropyl peroxydicarbonate, and initiator addition is the 2.5- of high polymer monomer weight
2.8%, prepolymerization time is 2-5 hours；
When high polymer monomer is the acrylic ester high molecular type monomer of refraction index 1.56, prepolymerization is at 45-50 DEG C
Carry out, initiator is di-isopropyl peroxydicarbonate, initiator addition is the 2.5-2.8% of high polymer monomer weight, in advance
Polymerization time is 2-5 hours；
When high polymer monomer is the acrylic ester high molecular type monomer of refraction index 1.60, prepolymerization is at 70-80 DEG C
Carry out, initiator is azo-bis-isobutyl cyanide, initiator addition is the 0.5-1.0% of high polymer monomer weight, prepolymerization time
It is 2-5 hours.
Another aspect, the present invention provides a kind of anti-blue light nanocomposite eyeglass, and it is using method system as described above
Make.
Another aspect, the present invention provides nano-composite resin material as described above and shows preparing blue light protection glass, LED
The application in the optical protective material fields such as screen protecting film, LED protecting film, automobile lamp, optical protection glass.
Hud typed transition metal oxide nano particle used in the present invention can be bought with market, such as Jiangsu Hua Tiantong
The hud typed transition metal oxide nano particle of Science and Technology Ltd.'s production, it is also possible to prepared according to known method, for example
Method disclosed in patent No. ZL96101878.X.Preferably, adopt and prepare hud typed transition metal oxide with the following method and receive
Rice corpuscles：
H is added dropwise in the transition metal salt solution for concentration being 0.1~1mol/L2SO4The aqueous solution to the transparent shape of solution, so
Alkaline aqueous solution is added dropwise afterwards makes precipitation settle out, and between 7-12, at 50 DEG C, acid adding dissolves precipitation to aqueous solution pH, obtains transition
The metal oxide hydrosol, pH adds surfactant and/or the ammoniacal liquor or sodium acetate as consisting of phase-transferring agent, transition between 1-7
Slaine, surfactant and the triangular molar ratio of consisting of phase-transferring agent are 1: (0.1-10): (0-1)；1-120 points of stirring
Clock, forms transition metal oxide cluster for core, the nano particle with coating material as shell；Through be dehydrated, dry loosely
Transition metal oxide nano particle.
The beneficial effects of the present invention are：Hud typed transition metal oxide (two is doped with resin lens of the invention
Titanium oxide, cobalt oxide and/or iron oxide) nano particle and ultra-violet absorber, by simple and effective manufacturing process, just may be used
Prepare the comprehensive and excellent high-performance anti-blue light resin lens of combination property.Nano particle is with ultra-violet absorber in resin base
Synergy is played in body assigns the nanocomposite eyeglass excellent anti-blue light performance, can high-efficient and lasting shielding wavelength exist
The high energy blue light and ultraviolet of the harm human eye of 380-450nm scopes.Additionally, nano-grade size and core shell structure cause nanometer
Grain has a splendid interface intermiscibility with macromolecule resin base material, thus its be uniformly dispersed in resin base material, good stability, tax
Give eyeglass clearly depending on thing and can distinguish the soft excellent optical property of color under strong and weak luminous environment.
Brief description of the drawings
Fig. 1 is 1.60 refractive index resin eyeglass anti-blue light Contrast on effect spectrograms.
Fig. 2 is different content TiO prepared by embodiment 12Anti-blue light PMMA/TiO2Resin sheet spectrogram.
Fig. 3 is different content TiO prepared by embodiment 22Anti-blue light PMS/TiO2Resin sheet spectrogram.
Fig. 4 is 1.49 refractive index different content TiO prepared by embodiment 52Anti-blue light resin lens spectrogram.
Fig. 5 is 1.56 refractive index different content TiO prepared by embodiment 62Anti-blue light resin lens spectrogram.
Fig. 6 is 1.60 refractive index different content TiO prepared by embodiment 72Anti-blue light resin lens spectrogram.
Specific embodiment
Design principle of the invention is as follows：
(1) protection wave-length coverage is determined
Medical research shows, human eye to the purple light of 380-450nm wave bands and some blue light are depending on thing and distinguish that color is insensitive, and
The short energy of wave band optical wavelength is high, big to eye injury.Ultraviolet is considered, it is determined that it is blue suitably to shield below 450nm
Light and ultraviolet, rational transmitance is kept to 450nm above sections blue light and visible ray.
Table 1：Anti-blue light resin sheet blue light protects wave-length coverage
| Wave-length coverage (nm) | Represent wavelength (nm) |
| 380-430 | 405 |
| 430-450 | 440 |
| 450-500 | 475 |
(2) anti-blue light resin material transmitance scope is designed
Wave-length coverage is protected according to the blue light formulated, makes anti-blue light resin material in ultraviolet and visible region representative wavelength
The peak transmittance at place reaches following table requirement：
The anti-blue light resin design of material transmitance of table 2
(3) determine the composition of transition metal oxide nano-particles and ultra-violet absorber in anti-blue light resin material, match somebody with somebody
Than and preparation condition.
Existing research shows, compared with pure resin base material, transition metal oxide nano-particles is mixed in resin base material
There are stronger absorption effects in 360-450nm afterwards, the light absorption range for mixing the resin base material of ultra-violet absorber is usually
360-410nm.Researcher of the invention has been surprisingly found that, when transition metal oxide nano-particles and the ultraviolet of proper proportion are inhaled
When receiving agent common distribution in resin base material, its absorbing wavelength is compared and individually mixes transition metal oxide nano-particles or ultraviolet
The wavelength of light absorbers produces red shift, as shown in figure 1, it is 2mm, 1.60 refractive index resin sheet material anti-blue light effects pair that it is thickness
Compare spectrogram.The present invention utilizes the synergy, the anti-blue light eyeglass transmitance scope formulated according to more than, to one or more
Transition metal oxide nano-particles and ultra-violet absorber compound and and resin compounded, preparing can high-efficiency shielding 380-
The blue light of 450nm scopes and whole ultraviolets, under strong and weak luminous environment can clearly depending on thing, distinguish that color is soft and wear-resisting and heat resistance
Excellent high-performance anti-blue light resin material and eyeglass.Research shows, is the resin material of 0.1-10mm for thickness, works as one kind
Or various nano-particle total amounts account for the 0.2%-2% of resin lens material gross weight, one or more ultra-violet absorber it is total
When amount accounts for the 0.5%-5% of resin lens material gross weight, the transmitance design model of above-mentioned blue light protection wavelength region is capable of achieving
Enclose.
Below by specific embodiment, the invention will be further described, but is not meant to the scope of the present invention
Limitation.
The hud typed transition metal oxide used in following examples is Jiangsu Huatiantong Technology Co., Ltd.'s production.
The particle diameter of the hud typed transition metal oxide nano-particles is 20-50nm；Its kernel is TiO2, CoO or Fe2O3；Shell is second
Sour natrium surfactant, thickness is 3-10nm.
Embodiment 1 prepares anti-blue light PMMA/TiO2Compound resin sheet material
Weigh 2.0g titanium dioxide nano-particles to be added in 100g methyl methacrylate monomers, magnetic agitation, disperse
Filtered through 0.45 μm of filter paper after uniform, add 2.0g ultra-violet absorbers (UV-328 and each 1.0g of UV-329), stirring mixing is equal
After even, initiator dibenzoyl peroxide 1.0g is added, stirring at low speed under 200r/min, control polymerisation 3 at 80 DEG C is small
When, complete prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing, the thickness of mould is 3mm, in solidification
85 DEG C were risen to from room temperature through 20 hours in stove, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, in accurate curing oven
120 DEG C of constant temperature 2 hours, completes secondary solidification, obtains the anti-blue light resin sheet containing nano-titania particle.
With above-mentioned same method, different TiO2 contents anti-blue light resin sheets are prepared, received with 0g titanium dioxide in step
Rice corpuscles replaces 2.0g titanium dioxide nano-particles, and accurate solidification temperature is by 105 DEG C of 120 DEG C of replacements.
Fig. 2 is equivalent ultraviolet radiation absorption agent content (2%) difference TiO2The anti-blue light PMMA/TiO of content2Resin sheet
Ultraviolet-visible spectrogram.As we know from the figure：Core-shell type nano TiO2Compound tree is assigned with the synergy of ultra-violet absorber
The excellent anti-blue light performance of fat sheet material, and in the case where ultraviolet radiation absorption dosage is fixed, increase nano-TiO2Content, resin
Sheet material increases in the absorption spectrum Einstein shift amount of ultraviolet visible light region, i.e. blue light absorption capability enhancing.Resin sheet is to more than 500nm
Visible light transmissivity is more than 83%.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 2 prepares anti-blue light PMS/TiO2Compound resin sheet material
Weigh the mix monomer that 2.0g titanium dioxide nano-particles are added to 10g methyl methacrylates and 90g styrene
In, magnetic agitation is filtered after being uniformly dispersed through 0.45 μm of filter paper, and (UV-326 is each with UV-327 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator azodiisobutyronitrile 1.0g is added, stirring at low speed under 200r/min is controlled at 80 DEG C
Lower polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould, the thickness of mould after 1 μm of strainer filtering, degassing
It is 3mm to spend, and 85 DEG C were risen to from room temperature through 20 hours in curing oven, completes one-step solidification；One-step solidification terminates, and die sinking is cleaned,
120 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the anti-blue light resin sheet containing nano-titania particle
Material.
With above-mentioned same method, different TiO are prepared2Content anti-blue light resin sheet, is received in step with 0g titanium dioxide
Rice corpuscles replaces 2.0g titanium dioxide nano-particles, and accurate solidification temperature is by 100 DEG C of 120 DEG C of replacements.
Fig. 3 is equivalent ultraviolet radiation absorption agent content (2%) difference TiO2The anti-blue light PMS/TiO of content2The purple of resin sheet
Outer visible light figure.As we know from the figure：Core-shell type nano TiO2Synergy with ultra-violet absorber assigns compound resin
The excellent anti-blue light performance of sheet material, and in the case where ultraviolet radiation absorption dosage is fixed, increase nano-TiO2Content, resin sheet
Material increases in the absorption spectrum Einstein shift amount of ultraviolet visible light region, i.e. blue light absorption capability enhancing.Resin sheet can to more than 500nm
See that light transmission rate is more than 81%.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 3 prepares anti-blue light PMS/TiO2Compound resin sheet material
Weigh the mix monomer that 2.0g titanium dioxide nano-particles are added to 50g methyl methacrylates and 50g styrene
In, magnetic agitation is filtered after being uniformly dispersed through 0.45 μm of filter paper, and (UV-326 is each with UV-327 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator azodiisobutyronitrile 1.0g is added, stirring at low speed under 200r/min is controlled at 80 DEG C
Lower polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould, the thickness of mould after 1 μm of strainer filtering, degassing
It is 3mm to spend, and 85 DEG C were risen to from room temperature through 20 hours in curing oven, completes one-step solidification；One-step solidification terminates, and die sinking is cleaned,
120 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the anti-blue light resin sheet containing nano-titania particle
Material.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 4 prepares anti-blue light PMS/TiO2Compound resin sheet material
Weigh the mix monomer that 2.0g titanium dioxide nano-particles are added to 90g methyl methacrylates and 10g styrene
In, magnetic agitation is filtered after being uniformly dispersed through 0.45 μm of filter paper, and (UV-326 is each with UV-327 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator azodiisobutyronitrile 1.0g is added, stirring at low speed under 200r/min is controlled at 80 DEG C
Lower polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould, the thickness of mould after 1 μm of strainer filtering, degassing
It is 3mm to spend, and 85 DEG C were risen to from room temperature through 20 hours in curing oven, completes one-step solidification；One-step solidification terminates, and die sinking is cleaned,
120 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the anti-blue light resin sheet containing nano-titania particle
Material.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 5 prepares 1.49 refractive index anti-blue light TiO2Compound resin eyeglass
Weigh the hud typed titanium dioxide nano-particles of 0.5g and be added to the diallyl diethylene glycol (DEG) that 100g refractive indexes are 1.49
In two carbonate monomers, magnetic agitation is filtered after being uniformly dispersed through 0.45 μm of filter paper, adds 2.0g ultra-violet absorbers (UV-
328 and each 1.0g of UV-329), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min
Stirring at low speed, control polymerisation 3 hours at 45 DEG C, completes prepolymerization；By pre-polymer mix through 1 μm of strainer filtering, degassing
After inject mould, rose to 85 DEG C from room temperature through 20 hours in curing oven, complete one-step solidification；One-step solidification terminates, and die sinking is washed
Only, 140 DEG C of constant temperature 2 hours in accurate curing oven, complete secondary solidification, obtain the anti-blue light resin containing nano-titania particle
Eyeglass, center thickness is 2mm.
With above-mentioned same method, different TiO are prepared2Content anti-blue light resin lens, are received in step with 0g titanium dioxide
Rice corpuscles, 1.0g titanium dioxide nano-particles, 2.0g titanium dioxide nano-particles replace 0.5g titanium dioxide nano-particles.
Fig. 4 is equivalent ultraviolet radiation absorption agent content (2%) difference TiO21.49 refractive index anti-blue light resin lens of content
Ultraviolet-visible spectrogram.As we know from the figure：Core-shell type nano TiO2Synergy with ultra-violet absorber assigns resin
The excellent anti-blue light performance of eyeglass, and in the case where ultraviolet radiation absorption dosage is fixed, with the increase of nanometer content, eyeglass exists
The absorption spectrum Einstein shift amount of ultraviolet visible light region increases, i.e. blue light absorption capability enhancing.Eyeglass is passed through to the visible above light of 500nm
Rate is more than 84%.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 6 prepares 1.56 refractive index anti-blue light TiO2Compound resin eyeglass
The hud typed titanium dioxide nano-particles of 0.5g are weighed to be added in the acrylate monomer that 100g refractive indexes are 1.56,
Magnetic agitation is simultaneously filtered after being uniformly dispersed through 0.45 μm of filter paper, and (UV-360 is each with UV-928 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min stirring at low speed, control are added
Polymerisation 3 hours at 50 DEG C, complete prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing,
85 DEG C were risen to from room temperature through 20 hours in curing oven, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, and solidifies in precision
140 DEG C of constant temperature 2.5 hours in stove, completes secondary solidification, obtains the anti-blue light resin lens containing titanium dioxide nano-particle, and center is thick
It is 2mm to spend.
With above-mentioned same method, different TiO are prepared2Content anti-blue light resin lens, are received in step with 0g titanium dioxide
Rice corpuscles, 1.0g titanium dioxide nano-particles, 2.0g titanium dioxide nano-particles replace 0.5g titanium dioxide nano-particles.
Fig. 5 is equivalent ultraviolet radiation absorption agent content (2%) difference TiO21.56 refractive index anti-blue light resin lens of content
Ultraviolet-visible spectrogram.As we know from the figure：Core-shell type nano TiO2Synergy with ultra-violet absorber assigns resin
The good anti-blue light performance of eyeglass, and in the case where ultraviolet radiation absorption dosage is fixed, with the increase of nanometer content, eyeglass exists
The absorption spectrum Einstein shift amount of ultraviolet visible light region increases, i.e. blue light absorption capability enhancing.Eyeglass is passed through to the visible above light of 500nm
Rate is more than 84%.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 7 prepares 1.60 refractive index anti-blue light TiO2Compound resin eyeglass
The hud typed titanium dioxide nano-particles of 0.5g are weighed to be added in the acrylate monomer that 100g refractive indexes are 1.60,
Magnetic agitation is simultaneously filtered after being uniformly dispersed through 0.45 μm of filter paper, and (UV-326 is each with UV-327 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator azodiisobutyronitrile 0.8g, 200r/min stirring at low speed is added, is controlled at 75 DEG C
Polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing, in curing oven
85 DEG C were risen to from room temperature through 20 hours, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, 140 DEG C in accurate curing oven
Constant temperature 3 hours, completes secondary solidification, obtains the anti-blue light resin lens containing titanium dioxide nano-particle, and center thickness is 2mm.
With above-mentioned same method, different TiO are prepared2Content anti-blue light resin lens, are received in step with 0g titanium dioxide
Rice corpuscles, 1.0g titanium dioxide nano-particles, 2.0g titanium dioxide nano-particles replace 0.5g titanium dioxide nano-particles.
Fig. 6 is equivalent ultraviolet radiation absorption agent content (2%) difference TiO21.60 refractive index anti-blue light resin lens of content
Ultraviolet-visible spectrogram.As we know from the figure：Core-shell type nano TiO2Synergy with ultra-violet absorber assigns resin
The good anti-blue light performance of eyeglass, and in the case where ultraviolet radiation absorption dosage is fixed, with the increase of nanometer content, eyeglass exists
The absorption spectrum Einstein shift amount of ultraviolet visible light region increases, i.e. blue light absorption capability enhancing.Eyeglass is passed through to the visible above light of 500nm
Rate is more than 80%.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 8 prepares 1.49 refractive index anti-blue light CoO compound resin eyeglasses
Weigh the hud typed cobalt oxide nanoparticles of 0.5g and be added to the diallyl diethylene glycol (DEG) two that 100g refractive indexes are 1.49
In carbonate monomer, magnetic agitation is simultaneously filtered after being uniformly dispersed through 0.45 μm of filter paper, adds 3.0g ultra-violet absorbers (UV-328
1.5g each with UV-329), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min low
Speed stirring, control polymerisation 3 hours at 45 DEG C, completes prepolymerization；By pre-polymer mix after 1 μm of strainer filtering, degassing
Injection mould, 85 DEG C were risen in curing oven through 20 hours from room temperature, completed one-step solidification；One-step solidification terminates, and die sinking is cleaned,
140 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the anti-blue light resin lens containing cobalt oxide nanoparticles,
Center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 9 prepares 1.56 refractive index anti-blue light CoO compound resin eyeglasses
Weigh the hud typed cobalt oxide nanoparticles of 1.0g to be added in the acrylate monomer that 100g refractive indexes are 1.56, magnetic
Power is stirred and filtered through 0.45 μm of filter paper after being uniformly dispersed, and (UV-360 is each with UV-928 to add 3.0g ultra-violet absorbers
1.5g), after being uniformly mixed, initiator di-isopropyl peroxydicarbonate 2.6g is added, stirring at low speed is controlled at 50 DEG C
Polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing, in curing oven
85 DEG C were risen to from room temperature through 20 hours, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, 140 DEG C in accurate curing oven
Constant temperature 2.5 hours, completes secondary solidification, obtains the anti-blue light resin lens containing cobalt oxide nanoparticles, and center thickness is 2mm.Can
Jian Guang areas transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 10 prepares 1.60 refractive index anti-blue light CoO compound resin eyeglasses
Weigh the hud typed cobalt oxide nanoparticles of 2.0g to be added in the acrylate monomer that 100g refractive indexes are 1.60, magnetic
Power is stirred and filtered through 0.45 μm of filter paper after being uniformly dispersed, and (UV-326 is each with UV-327 to add 3.0g ultra-violet absorbers
1.5g), after being uniformly mixed, initiator azodiisobutyronitrile 0.8g is added, stirring at low speed under 200r/min is controlled at 75 DEG C
Lower polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing, in curing oven
It is interior to rise to 85 DEG C from room temperature through 20 hours, complete one-step solidification；One-step solidification terminates, and die sinking is cleaned, 140 in accurate curing oven
DEG C constant temperature 3 hours, completes secondary solidification, obtains the anti-blue light resin lens containing cobalt oxide nanoparticles, and center thickness is 2mm.Can
Jian Guang areas transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 11 prepares 1.49 refractive index anti-blue light Fe2O3Compound resin eyeglass
Weigh the hud typed ferric oxide nano particles of 0.5g and be added to the diallyl diethylene glycol (DEG) two that 100g refractive indexes are 1.49
In carbonate monomer, magnetic agitation is simultaneously filtered after being uniformly dispersed through 0.45 μm of filter paper, adds 2.0g ultra-violet absorbers (UV-360
1.0g each with UV-928), after being uniformly mixed, add initiator di-isopropyl peroxydicarbonate 2.5g, 200r/min low
Speed stirring, control polymerisation 3 hours at 45 DEG C, completes prepolymerization；By pre-polymer mix after 1 μm of strainer filtering, degassing
Injection mould, 85 DEG C were risen in curing oven through 20 hours from room temperature, completed one-step solidification；One-step solidification terminates, and die sinking is cleaned,
140 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the anti-blue light resin lens containing ferric oxide nano particles,
Center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 12 prepares 1.56 refractive index anti-blue light Fe2O3Compound resin eyeglass
Weigh the hud typed ferric oxide nano particles of 1.0g to be added in the acrylate monomer that 100g refractive indexes are 1.56, magnetic
Power is stirred and filtered through 0.45 μm of filter paper after being uniformly dispersed, and (UV-360 is each with UV-928 to add 2.0g ultra-violet absorbers
1.0g), after being uniformly mixed, initiator di-isopropyl peroxydicarbonate 2.8g, 200r/min stirring at low speed, control are added
Polymerisation 3 hours at 50 DEG C, complete prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing,
85 DEG C were risen to from room temperature through 20 hours in curing oven, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, and solidifies in precision
140 DEG C of constant temperature 3 hours in stove, completes secondary solidification, obtains the anti-blue light resin lens containing ferric oxide nano particles, and center thickness is
2mm.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 13 prepares 1.60 refractive index anti-blue light Fe2O3Compound resin eyeglass
Weigh the hud typed ferric oxide nano particles of 1.5g to be added in the acrylate monomer that 100g refractive indexes are 1.60, magnetic
Power is stirred and filtered through 0.45 μm of filter paper after being uniformly dispersed, and (UV-326 is each with UV-327 to add 3.0g ultra-violet absorbers
1.5g), after being uniformly mixed, initiator azodiisobutyronitrile 0.8g, 200r/min stirring at low speed is added, is controlled at 75 DEG C
Polymerisation 3 hours, completes prepolymerization；Pre-polymer mix is injected into mould after 1 μm of strainer filtering, degassing, in curing oven
85 DEG C were risen to from room temperature through 20 hours, one-step solidification is completed；One-step solidification terminates, and die sinking is cleaned, 140 DEG C in accurate curing oven
Constant temperature 3 hours, completes secondary solidification, obtains the anti-blue light resin lens containing ferric oxide nano particles, and center thickness is 2mm.It can be seen that
Light area transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance the results are shown in Table 4.
Embodiment 14 prepares 1.49 refractive index anti-blue light nanocomposite eyeglasses
It is 1.49 to weigh 0.2g titanium dioxide, 0.2g cobalt oxides, 0.1g ferric oxide nano particles and be added to 100g refractive indexes
Diallyl diethylene glycol biscarbonate monomer in, magnetic agitation is simultaneously filtered after being uniformly dispersed through 0.45 μm of filter paper, adds 3.0g
Ultra-violet absorber (UV-360 and each 1.5g of UV-928), after being uniformly mixed, adds initiator peroxy dicarbonate two different
Propyl ester 2.5g, 200r/min stirring at low speed, control polymerisation 3 hours at 45 DEG C, completes prepolymerization；Pre-polymer mix is passed through
Mould is injected after 1 μm of strainer filtering, degassing, 85 DEG C were risen to from room temperature through 20 hours in curing oven, complete one-step solidification；Once
Solidification terminates, and die sinking is cleaned, 140 DEG C of constant temperature 2 hours in accurate curing oven, completes secondary solidification, obtains the nano-particle containing compounding
Anti-blue light resin lens, center thickness is 2mm.Visible region transmitance the results are shown in Table 3, and ultraviolet spectra area transmittance result is shown in
Table 4.
Embodiment 15：Anti-blue light resin lens transmitance test experience
Shanghai Yuan Xi Instrument Ltd. is selected in resin lens UV, visible light light transmission rate detection prepared by embodiment 1-10
UV-8000 type ultraviolet-visible photometers, as a result as shown in table 3, table 4.Result is learnt from table：Anti-blue light produced by the present invention
Eyeglass can effectively shield most of high energy blue light and whole ultraviolets of below 450nm, to the visible light transmissivity of more than 500nm
Higher than 80%.Eyeglass has the excellent clear property soft regarding thing, discoloration under strong and weak luminous environment while effective anti-blue light
Can, testing result is listed in the table below.
The anti-blue light resin lens visible region transmitance Eurya plant of table 3 surveys result
The anti-blue light resin lens ultraviolet spectra area transmittance testing result of table 4
Claims (10)
1. a kind of anti-blue light nano-composite resin material, it is characterised in that the material includes the high score for making optical material
Subtree fat and the hud typed transition metal oxide nano-particles and ultra-violet absorber that are scattered in macromolecule resin；Its
In, the macromolecule resin for making optical material is polymerized by high polymer monomer；Hud typed transition metal oxide is received
Rice corpuscles accounts for the 0.2%-2% of total resin weight, and ultra-violet absorber accounts for the 0.5%-5% of total resin weight；The ultraviolet
Absorbent be fat-soluble ultra-violet absorber, the fat-soluble ultra-violet absorber be UV-326, UV-327, UV-328, UV-329,
At least one in UV-360 and UV-928, mixes during using various ultra-violet absorbers according to arbitrary proportion.
2. anti-blue light nano-composite resin material as claimed in claim 1, it is characterised in that described for making optical material
Macromolecule resin be to be polymerized by high polymer monomer, the high polymer monomer is selected from：Vinyl monomer, epoxy resin high score
At least one in sub- monomer, polycarbonate-based high polymer monomer and polyurethane series high polymer monomer.
3. anti-blue light nano-composite resin material as claimed in claim 1, it is characterised in that the high polymer monomer is propylene
Acid esters type monomer or allylic monomers.
4. anti-blue light nano-composite resin material as claimed in claim 2 or claim 3, it is characterised in that the high polymer monomer choosing
From：Methyl methacrylate, styrene, refraction index are 1.49 diallyl diethylene glycol biscarbonate monomer, refraction index
For 1.56 acrylic ester high molecular type monomer and refraction index be in 1.60 acrylic ester high molecular type monomer at least one
Kind.
5. anti-blue light nano-composite resin material as claimed in claim 1, it is characterised in that the hud typed oxo transition metal
The particle diameter of compound nano-particle is 20-50nm；Its kernel is transition metal oxide, and the transition metal oxide is TiO2、CoO
And Fe2O3In at least one, during using more than one transition metal oxides according to arbitrary proportion mix；Shell is lived for surface
Property agent, thickness is 3-10nm；The surfactant is C2-C5Carboxylate, PVP or DBSA
Sodium.
6. the preparation method of the anti-blue light nano-composite resin material as any one of claim 1-5, it is characterised in that
The method comprises the following steps：
A. prepolymerization：Add in the high polymer monomer, hud typed transition metal oxide nano-particles and ultra-violet absorber
Enter initiator, heating carries out prepolymerization, obtains prepolymer；
B. after polymerization：The temperature programming of 10-20 hours will be carried out after above-mentioned prepolymer via hole diameter≤1 μm filter screen/membrane filtration
Solidification, solidification temperature rises to 85 DEG C from room temperature；Then solidify 2-6 hours at 100-160 DEG C, obtain anti-blue light optical resin material
Material.
7. a kind of anti-blue light nanocomposite eyeglass, it is characterised in that the resin lens are using any in claim 1-5
What the anti-blue light nano-composite resin material described in was made.
8. anti-blue light nanocomposite eyeglass as claimed in claim 7, it is characterised in that described hud typed in the eyeglass
Transition metal oxide nano-particles account for the 0.5%-2% of the total resin weight, and the ultra-violet absorber accounts for the resin
The 1%-3% of gross weight.
9. the preparation method of anti-blue light nanocomposite eyeglass as claimed in claim 7 or 8, it is characterised in that the method
Comprise the following steps：
A. the proportioning as described in claim 1 weighs high polymer monomer, the hud typed transition gold for preparing the macromolecule resin
Category oxide nano-particles and ultra-violet absorber；Hud typed transition metal oxide nano-particles are added to high polymer monomer
In, magnetic agitation makes nano-particle be dispersed in high polymer monomer, and via hole diameter≤0.45 μm filter paper/membrane filtration is standby；
B. prepolymerization：After adding ultra-violet absorber, stirring ultra-violet absorber to be completely dissolved in the mixed liquor that step A is obtained
Initiator is added, heating carries out prepolymerization, obtains prepolymer；
C. mold filling solidification：During above-mentioned prepolymer inserted into mould cavity after via hole diameter≤1 μm filter paper/membrane filtration, then will
It is put into the temperature programming carried out 15-20 hours in temperature programming stove and solidifies, and solidification temperature rises to 85 DEG C from room temperature；It is cooled to room
Die sinking, edging, cleaning after temperature；
D. two solidifications：The eyeglass that above-mentioned edging is cleaned is put into secondary curing oven, is solidified 2-3 hours at 120-140 DEG C, obtained
To optical resin lens.
10. method as claimed in claim 9, it is characterised in that in the prepolymerization of the step B,
When high polymer monomer is the diallyl diethylene glycol biscarbonate monomer of refraction index 1.49, prepolymerization is in 45-50
DEG C carry out, initiator is di-isopropyl peroxydicarbonate, initiator addition is the 2.5-2.8% of high polymer monomer weight,
Prepolymerization time is 2-5 hours；
When high polymer monomer is the acrylic ester high molecular type monomer of refraction index 1.56, prepolymerization is carried out at 45-50 DEG C,
Initiator is di-isopropyl peroxydicarbonate, and initiator addition is the 2.5-2.8% of high polymer monomer weight, during prepolymerization
Between be 2-5 hours；
When high polymer monomer is the acrylic ester high molecular type monomer of refraction index 1.60, prepolymerization is carried out at 70-80 DEG C,
Initiator is azo-bis-isobutyl cyanide, and initiator addition is the 0.5-1.0% of high polymer monomer weight, and prepolymerization time is 2-5
Hour.
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Address after: 211600 No. 73, Lishi Avenue, Jinhu Economic Development Zone, Huaian, Jiangsu Patentee after: New material Limited by Share Ltd of Jiangsu University of optic science Address before: 211600 No. 73, Lishi Avenue, Jinhu Economic Development Zone, Huaian, Jiangsu Patentee before: JIANGSU SHIKE NEW MATERIAL CO., LTD. |