CN103487848A - Colorless and transparent resin lens containing cobaltous oxide nanometer material and manufacturing method thereof - Google Patents
Colorless and transparent resin lens containing cobaltous oxide nanometer material and manufacturing method thereof Download PDFInfo
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- CN103487848A CN103487848A CN201210192599.4A CN201210192599A CN103487848A CN 103487848 A CN103487848 A CN 103487848A CN 201210192599 A CN201210192599 A CN 201210192599A CN 103487848 A CN103487848 A CN 103487848A
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Abstract
The invention relates to a colorless and transparent resin lens containing cobaltous oxide nanometer material. Cobaltous oxide nano-particles of core-shell structures are mingled into the lens. According to a manufacturing method of the colorless and transparent resin lens containing cobaltous oxide nanometer material, the cobaltous oxide nano-particles of the core-shell structures are dispersed and dissolved in polymer monomers, the mixture is filtered, an initiator is added into the mixed liquor, a color matching agent is added into the mixed liquor to adjust the mixed liquor to be colorless, the mixed liquor is heated to undergo polymerization reaction, and then a prepolymer is obtained; the prepolymer is filled into a cavity of a mold after being filtered, the mold is placed into a temperature programming oven to be cured through 15-20 hours of temperature programming, and then mold opening, edge polishing and washing are performed; the washed lens with the edges polished is placed into a secondary curing oven, cured for 2-3 hours at 120-140 DEG C, and the optical resin lens is obtained. The resin lens manufactured with the method is high in light transmittance, good in visuality and excellent in wearing resistance and heat resistance.
Description
Technical field
The invention belongs to a kind of colourless resin optical lens, particularly containing the resin optical lens of cobalt oxide nano particle.
Background technology
Since resin lens is born, how manufacturer always allows the usability of light, saturating resin lens further get a promotion if being pursued.But owing to being that the macromolecule resin material skin hardness is lower, wear no resistance, often need the multiple working procedures such as stiffened, plated film in manufacture process.
The characteristic spectrum of transition metal oxide nano-material absorbs, make it can shield gamma-rays, X ray, ultraviolet ray, see through selectively or the absorption portion visible ray, see through selectively or the absorption portion infrared ray, therefore, the existing considerable application prospect in the optical material field.But, because inorganic material is dispersed poor in macromolecule resin material, restrict the application of transition metal oxide nano-material in the optical mirror slip field always.
Summary of the invention
For the problems referred to above of prior art, the invention provides a kind of colourless transparent resin eyeglass containing the cobalt oxide nano material and preparation method thereof.This titanium dioxide nano material is nucleocapsid structure, and its outside coating material layer has the intermiscibility good with macromolecule resin material, and nano particle is evenly distributed in the macromolecule grid, effectively improves fastness to rubbing, transmittance, thermotolerance of resin lens etc.
For achieving the above object, the present invention includes following technical scheme:
A kind of colourless transparent resin eyeglass containing the cobalt oxide nano material, the nucleocapsid structure cobalt oxide nano particle that it comprises the macromolecule resin for making optical mirror slip and is doped in macromolecule resin; Wherein, the particle diameter of this nucleocapsid structure cobalt oxide nano particle is 20-50nm, and kernel is the cobalt oxide particle, and shell is coating material.
Colourless transparent resin eyeglass containing the cobalt oxide nano material as above, preferably, the 0.005-0.025% that the amount of described nucleocapsid structure cobalt oxide nano particle is this macromolecule resin general assembly (TW).
Colourless transparent resin eyeglass containing the cobalt oxide nano material as above, preferably, described is to be polymerized by following high polymer monomer for the macromolecule resin of making optical mirror slip: the acrylic ester high molecular type monomer that the acrylic ester high molecular type monomer (abbreviation rolls over 1.56) that the diglycol allyl carbonate monomer that refraction index is 1.499 (being called for short CR39), refraction index are 1.56 and/or refraction index are 1.61.
Colourless transparent resin eyeglass containing the cobalt oxide nano material as above, preferably, prepared by described nucleocapsid structure cobalt oxide nano particle by the following method:
In the cobalt salt solution that is 0.1～10mol/L to concentration, drip alkaline aqueous solution and make to settle out, aqueous solution pH is between 7-12; Under 45-55 ℃, acid adding is dissolved precipitation, obtains cobalt oxide hydrosol pH between 3-5; Add as the C2-C5 carboxylate of coating material or sodium dodecyl benzenylsulfonate and/or as ammoniacal liquor or the sodium acetate of consisting of phase-transferring agent, the triangular mol ratio of cobalt salt, coating material and consisting of phase-transferring agent is 1: (0.1-10): (0-1), stir 10-60 minute, have nano oxidized cobalt granule to generate; By solution through centrifugal dehydration, dry to obtain nucleocapsid structure cobalt oxide nano particle.
Colourless transparent resin eyeglass containing the cobalt oxide nano material as above, preferably, described cobalt salt is cobaltous sulphate, cobalt nitrate or cobalt chloride.
On the other hand, the present invention also comprises the manufacture method of the colourless transparent resin eyeglass containing the cobalt oxide nano material as above, and the method comprises the steps:
A. take described nucleocapsid structure cobalt oxide nano material and, for making the high polymer monomer of optical mirror slip, cobalt oxide nano material dispersing and dissolving, in high polymer monomer, filtered;
B. prepolymerization: add initiating agent in the mixed liquor obtained to steps A, add subsequently the resin lens toner that the mixed liquor color is adjusted into colourless, polyreaction is carried out in heating, obtains prepolymer;
C. mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, subsequently mould is put into to the temperature programme that the temperature programme stove carries out 15-20 hour and solidified, solidification temperature rises to 85 ℃ from room temperature; Be cooled to room temperature, die sinking subsequently, edging, clean;
D. regelate: by above-mentioned edging, clean eyeglass is put into the regelate stove, at 120-140 ℃ of curing 2-3 hour, obtains optical resin lens.
Method as above, preferably, in the prepolymerization of described step B, the diglycol allyl carbonate monomer polymerization reactions that refraction index is 1.499 carries out at 45-50 ℃, initiating agent is the diisopropyl peroxy carbonates, the 2.5-2.8% that the initiating agent addition is high polymer monomer weight, polymerization time is 2-5 hour.
Method as above, preferably, in the prepolymerization of described step B, the acrylic ester high molecular type monomer polymerization reactions that refraction index is 1.56 carries out at 45-50 ℃, initiating agent is the diisopropyl peroxy carbonates, the 2.5-2.8% that the initiating agent addition is high polymer monomer weight, polymerization time is 2-5 hour.
Method as above, preferably, in the prepolymerization of described step B, the acrylic ester high molecular type monomer that refraction index is 1.61 carries out polymerization at 70-80 ℃, initiating agent is azo two cyanogen in different heptan, the 0.5-1.0% that the initiating agent addition is high polymer monomer weight, polymerization time is 2-5 hour.
Method as above, preferably, described resin lens toner is blue ultramarine and/or red ultramarine.
Again on the one hand, the present invention includes a kind of colourless transparent resin eyeglass containing the cobalt oxide nano material, it is applied method as mentioned above and manufactures.
Beneficial effect of the present invention is: the nucleocapsid structure cobalt oxide nano composite material of having adulterated in resin lens of the present invention.This nano composite material, except the favorable optical performance that the cobalt oxide nano particle has, because shell has coating material, therefore has splendid interface phase dissolubility in macromolecule resin material, can improve dispersiveness, stability and the mechanical property of product.Therefore, colourless transparent resin eyeglass wearing quality, transmitance, the fine heat-resisting performance of using method of the present invention to manufacture.In the situation that optical transmittance anti-wear performance identical with the commercial resins eyeglass is 3 times (the wearing quality data are from national eyewear products quality supervision and test centers) of commercially available colourless transparent resin eyeglass, thermal property also improves a lot, commercially available colourless resin eyeglass usually in accurate curing oven 140 ℃ solidify 2 hours eyeglasses crackings and flavescence, the eyeglass containing nano material of the present invention carries out at 140-160 ℃ the not flavescence of not ftractureing after regelate in 2 hours.Simultaneously, due to cobalt oxide nano material itself, with color, adding the Polymer Solution after initiating agent is light green color, through the color toner bleaching, thereby can obtain the water white transparency optical mirror slip of containing metal oxide nano material.
Embodiment
Embodiment 1 prepares nucleocapsid structure cobalt oxide nano particle
In the cobalt sulfate solution that is 1mol/L to 1000mL concentration, drip the NaOH aqueous solution and make to settle out, aqueous solution pH, between 8-9, under 50 ℃, adds hydrochloric acid precipitation is dissolved, and obtains the cobalt oxide hydrosol, and pH is 3-4.Add the Sodium butyrate aqueous solution 100mL that concentration is 2mol/L, after stirring 40 minutes, have nano oxidized cobalt granule to generate, through separating and dehydrating, dry to constant weight under 50 ℃, obtain the cobalt oxide nano particle of nucleocapsid structure, particle diameter is 20-50nm.
Embodiment 2
Prepare the colourless transparent resin optical lens according to following steps:
(1) preparation of toner solution: the blue ultramarine of 0.16 gram (commercially available) is added in 1 kilogram of high polymer monomer CR39, the red ultramarine of 0.3 gram (commercially available) is added to 1 kilogram of high polymer monomer CR39.
(2) prepolymerization: by the cobalt oxide nano material dispersing and dissolving of embodiment 1 preparation, in the CR39 high polymer monomer, the nano material addition is 0.012% of high polymer monomer weight.Through filtering, (chemical name: 2-hydroxyl-4 octyloxy benzophenone), the ultraviolet light absorber addition is 0.03% of high polymer monomer weight to add commercially available ultraviolet light absorber UV531.Add subsequently initiating agent diisopropyl peroxy carbonates, the initiating agent addition is 2.8% of high polymer monomer weight.Thereafter the toner solution that adds step (1) to prepare, it is 0.300% of high polymer monomer weight that toner solution adds total amount, blue and red ratio is 2: 1.Within 3 hours, obtain prepolymer 45 ℃ of polyreactions.
(3) mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, put into the temperature programme that the temperature programme stove carries out 17 hours and solidify, temperature range 20-85 ℃; Be cooled to room temperature, mould is opened, take out the resin optical lens edging, clean.
(4) regelate moulding: solidify 2 hours in 140 ℃ in accurate curing oven, be cooled to room temperature, obtain resin optical lens.
After tested, this eyeglass is up to 92% left and right in the visible region transmitance, reaches 96-98% after plated film.Anti-wear performance: friction number of times 5000, assay, wearing quality 5.61% (the anti-wear performance data are from national eyewear products quality supervision and test center survey report).Thermal property: eyeglass carries out cracking, flavescence not occurring after regelate in 2 hours at 140-160 ℃.
Comparing embodiment 1
Except not adding in high polymer monomer the cobalt oxide nano material, adopt the method identical with embodiment 2 to prepare resin lens.
After tested, this lens optical is up to 92% left and right in the visible region transmitance, reach 96-98% after plated film, anti-wear performance: friction number of times 5000, assay, wearing quality 15.72%, (wear-resisting data are from national eyewear products quality supervision and test center survey report), this colourless resin eyeglass ftractures and flavescence at 2 hours eyeglasses of 140 ℃ of heating.
Embodiment 3
Prepare the colourless transparent resin optical lens according to following steps:
(1) prepolymerization: by the cobalt oxide nano material dispersing and dissolving (CR39) in high polymer monomer of embodiment 1 preparation, the nano material addition is 0.024% of high polymer monomer weight, through filtering, add commercially available ultraviolet light absorber UV531, the ultraviolet light absorber addition is 0.03% of monomer weight, add subsequently initiating agent diisopropyl peroxy carbonates, the initiating agent addition is 2.8% of monomer weight.Thereafter add toner solution as described in Example 2, it is 0.335% of high polymer monomer weight that toner solution adds total amount, blue and red ratio 1.5: 1.Within 3 hours, obtain prepolymer 45 ℃ of polyreactions.
(2) mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, put into the temperature programme that the temperature programme stove carries out 17 hours and solidify, solidification temperature is from room temperature to 85 ℃.Be cooled to room temperature, mould is opened, take out the resin optical lens edging, clean.
(3) regelate moulding: solidify 2 hours at 140 ℃ in accurate curing oven, be cooled to room temperature, obtain resin optical lens.
After tested, this lens optical is up to 92% left and right in the visible region transmitance, reaches 96-98% after plated film.Anti-wear performance: friction number of times 5000, assay, wearing quality 4.72% (wear-resisting data are from national eyewear products quality supervision and test center survey report).Thermal property: eyeglass carries out regelate at 140-160 ℃ and cracking, flavescence within 2 hours, do not occur.
Embodiment 4
Prepare the colourless transparent resin optical lens according to following steps:
(1) prepolymerization: by the transiting metal oxidation cobalt nano material dispersing and dissolving (middle folding 1.56) in high polymer monomer of embodiment 1 preparation, the nano material addition is 0.020% of high polymer monomer weight.Through filtration, add commercially available ultraviolet light absorber UV531, the ultraviolet light absorber addition is 0.03% of monomer weight.Add initiating agent diisopropyl peroxy carbonates, the initiating agent addition is 2.8% of monomer weight.Add subsequently toner solution as described in Example 2, toner solution addition is 0.40% of high polymer monomer weight, blue and red ratio 1.5: 1.Within 3 hours, obtain prepolymer 75 ℃ of polyreactions.
(2) mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, put into the temperature programme that the temperature programme stove carries out 17 hours and solidify, solidification temperature rises to 85 ℃ from room temperature.Be cooled to room temperature, mould is opened, take out the resin optical lens edging, clean.
(3) regelate moulding: solidify 2 hours in 140 ℃ in accurate curing oven, be cooled to room temperature, obtain resin optical lens.
After tested, this lens optical is up to 92% left and right in the visible region transmitance, reaches 96-98% after plated film.Anti-wear performance: friction number of times 5000, assay, wearing quality 4.921%.Thermal property: eyeglass carries out regelate at 140-160 ℃ and cracking, flavescence within 2 hours, do not occur.
Embodiment 5
Prepare the colourless transparent resin optical lens according to following steps:
(1) prepolymerization: in the acrylic ester high molecular type monomer that is 1.61 in refraction index by the transiting metal oxidation cobalt nano material dispersing and dissolving of embodiment 1 preparation, the nano material addition is 0.025% of high polymer monomer weight, through filtering, add commercially available ultraviolet light absorber UV531, the ultraviolet light absorber addition is 0.03% of monomer weight.Add initiating agent azo two cyanogen in different heptan, the initiating agent addition is 1.0% of monomer weight.Add subsequently toner solution as described in Example 2, toner solution addition is 0.45% of high polymer monomer weight, blue and red ratio 1.5: 1.Within 3 hours, obtain prepolymer 75 ℃ of polyreactions.
(2) mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, put into the temperature programme that the temperature programme stove carries out 17 hours and solidify, solidification temperature rises to 85 ℃ from room temperature.Be cooled to room temperature, mould is opened, take out the resin optical lens edging, clean.
(3) regelate moulding: solidify 2 hours in 140 ℃ in accurate curing oven, be cooled to room temperature, obtain resin optical lens.
After tested, this lens optical is up to 92% left and right in the visible region transmitance, reaches 96-98% after plated film.Anti-wear performance: friction number of times 5000, assay, wearing quality 4.120%.Thermal property: eyeglass carries out regelate at 140-160 ℃ and cracking, flavescence within 2 hours, do not occur.
Claims (9)
1. the colourless transparent resin eyeglass containing the cobalt oxide nano material, is characterized in that the nucleocapsid structure cobalt oxide nano particle that it comprises the macromolecule resin for making optical mirror slip and is doped in macromolecule resin; Wherein, the particle diameter of this nucleocapsid structure cobalt oxide nano particle is 20-50nm, and kernel is the cobalt oxide particle, and shell is coating material.
2. the colourless transparent resin eyeglass containing the cobalt oxide nano material as claimed in claim 1, is characterized in that the 0.005-0.025% that the amount of described nucleocapsid structure cobalt oxide nano particle is this macromolecule resin general assembly (TW).
3. the colourless transparent resin eyeglass containing the cobalt oxide nano material as claimed in claim 1, it is characterized in that, described is to be polymerized by following high polymer monomer for the macromolecule resin of making optical mirror slip: the acrylic ester high molecular type monomer that the diglycol allyl carbonate monomer that refraction index is 1.499, the acrylic ester high molecular type monomer that refraction index is 1.56 and/or refraction index are 1.61.
4. the colourless transparent resin eyeglass containing the cobalt oxide nano material as claimed in claim 1, is characterized in that, prepared by the following method by described nucleocapsid structure cobalt oxide nano particle:
In the cobalt salt solution that is 0.1～10mol/L to concentration, drip alkaline aqueous solution and make to settle out, aqueous solution pH is between 7-12; Under 45-55 ℃, acid adding is dissolved precipitation, obtains cobalt oxide hydrosol pH between 3-5; Add as the C2-C5 carboxylate of coating material or sodium dodecyl benzenylsulfonate and/or as ammoniacal liquor or the sodium acetate of consisting of phase-transferring agent, the triangular mol ratio of cobalt salt, coating material and consisting of phase-transferring agent is 1: (0.1-10): (0-1), stir 10-60 minute, have nano oxidized cobalt granule to generate; By solution through centrifugal dehydration, dry to obtain nucleocapsid structure cobalt oxide nano particle.
5. the colourless transparent resin eyeglass containing the cobalt oxide nano material as claimed in claim 4, is characterized in that, described cobalt salt is cobaltous sulphate, cobalt nitrate or cobalt chloride.
6. the manufacture method of the colourless transparent resin eyeglass containing the cobalt oxide nano material as described as any one in claim 1-5, is characterized in that, the method comprises the steps:
A. take described nucleocapsid structure cobalt oxide nano material and, for making the high polymer monomer of optical mirror slip, cobalt oxide nano material dispersing and dissolving, in high polymer monomer, filtered;
B. prepolymerization: add initiating agent in the mixed liquor obtained to steps A, add subsequently the resin lens toner that the mixed liquor color is adjusted into colourless, polyreaction is carried out in heating, obtains prepolymer;
C. mold filling solidifies: above-mentioned prepolymer is inserted in mould cavity after filtering, subsequently mould is put into to the temperature programme that the temperature programme stove carries out 15-20 hour and solidified, solidification temperature rises to 85 ℃ from room temperature; Be cooled to room temperature, die sinking subsequently, edging, clean;
D. regelate: by above-mentioned edging, clean eyeglass is put into the regelate stove, at 120-140 ℃ of curing 2-3 hour, obtains optical resin lens.
7. method as claimed in claim 6, it is characterized in that, in the prepolymerization of described step B, the diglycol allyl carbonate monomer polymerization reactions that refraction index is 1.499 carries out at 45-50 ℃, initiating agent is the diisopropyl peroxy carbonates, the 2.5-2.8% that the initiating agent addition is high polymer monomer weight, polymerization time is 2-5 hour; The acrylic ester high molecular type monomer polymerization reactions that refraction index is 1.56 carries out at 45-50 ℃, and initiating agent is the diisopropyl peroxy carbonates, the 2.5-2.8% that the initiating agent addition is high polymer monomer weight, and polymerization time is 2-5 hour; The acrylic ester high molecular type monomer that refraction index is 1.61 carries out polymerization at 70-80 ℃, and initiating agent is azo two cyanogen in different heptan, the 0.5-1.0% that the initiating agent addition is high polymer monomer weight, and polymerization time is 2-5 hour.
8. method as claimed in claim 7, is characterized in that, described resin lens toner is blue ultramarine and/or red ultramarine.
9. the colourless transparent resin eyeglass containing the cobalt oxide nano material, is characterized in that, it is applied method as claimed in claim 6 and manufactures.
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| CN201210192599.4A CN103487848B (en) | 2012-06-12 | 2012-06-12 | Colourless transparent resin eyeglass containing cobalt oxide nano material and manufacture method thereof |
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Cited By (8)
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| CN103837920A (en) * | 2014-03-18 | 2014-06-04 | 江苏华天通科技有限公司 | Filter lens for electric welding and method for manufacturing filter lens for electric welding |
| CN103980643A (en) * | 2014-06-04 | 2014-08-13 | 江苏华天通纳米科技有限公司 | Blue light cut nano compound resin material, lens and preparation method thereof |
| CN103992422A (en) * | 2014-06-04 | 2014-08-20 | 江苏华天通纳米科技有限公司 | Anti-blue light nanometer composite monomer material and anti-blue light optical resin prepared from same |
| CN105754275A (en) * | 2016-02-25 | 2016-07-13 | 侯绪华 | Anti-blue light no-coated lens of glasses |
| CN108788126A (en) * | 2018-06-20 | 2018-11-13 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN108948625A (en) * | 2018-07-27 | 2018-12-07 | 望江县天长光学科技有限公司 | A kind of optical resin lens of the nano material containing cobalt oxide |
| CN114031818A (en) * | 2021-10-25 | 2022-02-11 | 江苏视科新材料股份有限公司 | Organic/inorganic nano composite microsphere visual light material and application thereof |
| CN115286746A (en) * | 2022-07-18 | 2022-11-04 | 江苏可奥熙光学材料科技有限公司 | Resin monomer suitable for wear-resistant lens with refractive index of 1.56 and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103837920A (en) * | 2014-03-18 | 2014-06-04 | 江苏华天通科技有限公司 | Filter lens for electric welding and method for manufacturing filter lens for electric welding |
| CN103980643A (en) * | 2014-06-04 | 2014-08-13 | 江苏华天通纳米科技有限公司 | Blue light cut nano compound resin material, lens and preparation method thereof |
| CN103992422A (en) * | 2014-06-04 | 2014-08-20 | 江苏华天通纳米科技有限公司 | Anti-blue light nanometer composite monomer material and anti-blue light optical resin prepared from same |
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| CN105754275A (en) * | 2016-02-25 | 2016-07-13 | 侯绪华 | Anti-blue light no-coated lens of glasses |
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| CN108788126A (en) * | 2018-06-20 | 2018-11-13 | 陕西理工大学 | A kind of preparation method of cobalt nano magnetic material |
| CN108948625A (en) * | 2018-07-27 | 2018-12-07 | 望江县天长光学科技有限公司 | A kind of optical resin lens of the nano material containing cobalt oxide |
| CN114031818A (en) * | 2021-10-25 | 2022-02-11 | 江苏视科新材料股份有限公司 | Organic/inorganic nano composite microsphere visual light material and application thereof |
| CN115286746A (en) * | 2022-07-18 | 2022-11-04 | 江苏可奥熙光学材料科技有限公司 | Resin monomer suitable for wear-resistant lens with refractive index of 1.56 and preparation method thereof |
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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. |
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