CN102660115B - Combination for preparing lens with good safety and preparation method of lens - Google Patents
Combination for preparing lens with good safety and preparation method of lens Download PDFInfo
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- CN102660115B CN102660115B CN201210161913.2A CN201210161913A CN102660115B CN 102660115 B CN102660115 B CN 102660115B CN 201210161913 A CN201210161913 A CN 201210161913A CN 102660115 B CN102660115 B CN 102660115B
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Abstract
The invention mainly relates to a combination for preparing a resin lens with good safety. The combination is prepared by adopting diisocyanate, polyatomic alcohol, catalyst and ultraviolet absorber, an internal release agent and a color matching agent according to formula dose; and the invention also relates to a method for preparing the resin lens by utilizing the combination. The prepared resin lens has the advantages of being high in hardness, light in mass and radiation resistant, and can meet the requirements of glass wearers on safety and comfortableness.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of for the preparation of security good eyeglass composition and utilize said composition to prepare the method for eyeglass.
Background technology
According to statistics, global myopia accounts for 30%~40% of total number of persons, so glasses become people's the requisite articles for use of daily life greatly.Eyeglass is the key part of glasses, and the quality of its performance will directly affect the result of use of glasses.Before reaching the nineties in last century, glasses lens generally adopts glass material, and the eyeglass of glass material is often frangible, heavier, has greatly affected security and the comfortableness of myope's wearing spectacles, therefore by resin lens, is replaced gradually.
Current ordinary resin eyeglass is to adopt glycol ether propenyl carbonic ether (ADC) material polymerization manufacture to form or adopt the eyeglass of diallyl isophthalate, diallyl p phthalate, dibutyl maleinate and ADC monomer copolymerization, and patent documentation CN1548988A, CN101017209A, CN101778879, CN1910503A etc. all have disclosure in various degree.But these eyeglasses hardness often are inadequate, easily broken, bring certain potential safety hazard to eyeglass wearer, although have improved to a certain extent hardness, eyeglass is very heavy, has affected the comfort level of wearing.In addition, in the resin lens industry, for the minimum requirements of expressing the eyeglass with safety performance and must meet U.S. FDA regulation, its requirement is that the steel ball that weight reaches 16.8g freely falls to testing lens from the 127cm eminence, and eyeglass must be not damaged.The eyeglass of above-mentioned materials its shock-resistance after the stiffened that improves optical property and antireflection film layer are processed is subject to larger deteriorated, can not meet the minimum requirements of FDA, therefore do not there is security, and the mechanical property of these eyeglasses is poor, often occurs breakage when eyeglass is ground.
Therefore develop the eyeglass that a kind of hardness is high, quality is light very necessary.
Summary of the invention
The present invention mainly is to provide a kind of composition of, eyeglass that quality light high for the preparation of hardness, and utilizes this kind of composition preparation to have the method for above-mentioned premium properties eyeglass.
At first the present invention provides a kind of composition for the manufacture of resin lens, and the component of said composition and degree by weight are:
Vulcabond 0-60%
Polyvalent alcohol 40-70%;
The additive that surplus is following component and content,
Catalyzer 50-2000 ppm
UV light absorber 300-20000 ppm
Inner pattern releasing agent applicable 0-5000 ppm
Toning agent 0-50 ppm;
The content sum of above each component is 100%.
Those of ordinary skill in the art should know ppm(parts per million) what mean is to account for by the solute quality concentration that the part per million of complete soln quality means, also claims ppm, lower together.
Preferably, vulcabond in the composition of described manufacture resin lens is 3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate, hexamethylene vulcabond, HMDI, 1,3-bis-(isocyanic ester methyl) benzene, one or more in two (isocyanic ester methyl) hexanaphthene, 2,5 (2,6)-bis-(isocyanic ester methyl) two ring [2.2.1] heptane or Methylcyclohexyl diisocyanate.Further preferably, described vulcabond is 3-isocyanic ester methylene-3,5, one or more in 5-3-methyl cyclohexanol based isocyanate, hexamethylene vulcabond and HMDI.
Preferably, the polyvalent alcohol in the composition of described manufacture resin lens be four (3-thiohydracrylic acid) pentaerythritol ester, four (Thiovanic acid) pentaerythritol esters, four (3-thiohydracrylic acid) trihydroxymethylpropanyl ester, tri-thiol acetic acid trihydroxymethylpropanyl ester or four Thiovanic acid two (TriMethylolPropane(TMP)) esters or in one or more.Further preferably, described polyvalent alcohol is four (3-thiohydracrylic acid) pentaerythritol ester and/or four (Thiovanic acid) pentaerythritol esters.
Preferably,
Catalyzer in the composition of described manufacture resin lens is amine, or dibutyl tin dichloride, dibutyl tin laurate, dibutyltin diacetate, stannous octoate, dibutyl tin laurate, tin tetrafluoride, tin tetrachloride, tin tetrabromide, tin tetraiodide, methyl tin chloride, dimethyl chlorination tin, dibutyl tin oxide, dibutyltin chloride, tributyltin chloride, fentin chloride, dibutyl tin thioether, two (2-(ethylhexyl)) one or more in tin-oxide;
Described UV light absorber is the tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole, 2-(3 '-tertiary butyl-2 '-hydroxyl-5 '-aminomethyl phenyl)-5-chlorobenzotriazole, 2-(2 '-hydroxyl-3 ' 5 '-di-tert-butyl-phenyl)-5-chlorobenzotriazole, 2-(2'-hydroxyl-5'-aminomethyl phenyl) benzotriazole, 2,4-dihydroxy benaophenonel, ESCALOL 567,2-hydroxyl-4-benzyloxy benzophenone, 2, one or more in 2 '-dihydroxyl-4-methoxy benzophenone and 2-dihydroxyl-4-oxy-octyl benzophenone;
Described inner pattern releasing agent applicable is fluorine-containing nonionic surface active agent, siliceous tensio-active agent, quaternary ammonium alkyl, acid phosphoric acid ester, poly-methyl-silicone oil, poly-ethyl silicon oil and polymethylphenyl siloxane fluid; More preferably, described inner pattern releasing agent applicable acid phosphoric acid ester class releasing agent is as p isopropylbenzoic acid ester, diisopropyl phosphate, butyl phosphate, octyl phosphate, dioctylphosphoric acid ester, phosphoric acid isodecyl ester, di(2-ethylhexyl)phosphate isodecyl ester, phosphoric acid tridecyl ester, di(2-ethylhexyl)phosphate (tridecyl) ester or be their mixture; In addition also, can make the ZELEC UN phosphoric acid ester releasing agent of U.S. Si Taipan (STEPAN) company;
The aminoketones dyestuff of the dyestuff that described toning agent is anthraquinone type and heterocyclic type.
The present invention also provides the method for utilizing above-mentioned composition to manufacture resin lens, and the method comprises the steps:
(1) monomer of formula ratio is added in the reactor of sealing, use dry nitrogen replacement to fall air;
(2) mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with the 0.5-5 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Room temperature---35 ℃ 0.5 hour
35 ℃---35 ℃ 1 hour
35 ℃---40 ℃ 2 hours
40 ℃---60 ℃ 3 hours
60 ℃---60 ℃ 4 hours
60 ℃---120 ℃ 7 hours
120 ℃---120 ℃ 2 hours
120 ℃---70 ℃ 1 hour
(3) remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 100-120 degree centigrade is processed.
Preferably, the method for above-mentioned manufacture resin lens, the method also comprises that methods such as adopting dip-coating, spin coating or spraying adopt to be heating and curing and form the hard coat that adds of 0.5-5 micron thick on eyeglass.Further preferably, the described hard coat that adds is by the mixture of the Nano sol of the organo-silicon coupling agent hydrolyzate with epoxide group and silicon-dioxide, zirconium dioxide, titanium dioxide, aluminum oxide, stannic oxide, niobium oxides.
Preferably, the method for above-mentioned manufacture resin lens, the method also comprises the rete of evaporation one deck fluoro-resin.
To the test of testing of the above-mentioned eyeglass made, result shows:
the specific refractory power of eyeglass is 1.54~1.56, and the transmittance of the eyeglass of processing through antireflective coating is greater than 98%;
the ultraviolet filtering that the plano lens wavelength that thickness is 2.0mm is less than or equal to 400nm is greater than 99%.
Therefore, the eyeglass that utilizes above-mentioned composition and method to prepare, have that hardness is high, quality is light, radiation-resistant advantage, can meet the requirement of eyeglass wearer to security and comfortableness.
Embodiment
Below in conjunction with specific embodiment, content of the present invention is further elaborated.
embodiment 1 composite formula and eyeglass preparation technology
(1) fill a prescription 1:
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 200 grams
Hexamethylene vulcabond 250 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 550 grams
Dichloride dibutyl tin 1.2 grams
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 15 grams
Zelecun
1 gram
Solvent violet dyestuff 0.5 gram
(2) preparation technology:
Monomer is added in the reactor of sealing after 1 weighing by formula, use dry nitrogen replacement to fall air.Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Reactions steps | Temperature of reaction | Reaction times |
1) | Room temperature---35 ℃ | 0.5 hour |
2) | 35℃ | 1 hour |
3) | 35℃---40℃ | 2 hours |
4) | 40℃---60℃ | 3 hours |
5) | 60℃ | 4 hours |
6) | 60℃---120℃ | 7 hours |
7) | 120℃ | 2 hours |
8) | 120℃---70℃ | 1 hour |
Then remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 100-120 degree is processed.
Prepared eyeglass, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
(3) performance test
Adopt the method for ISO8980.3-2004 " burr glasses lens (third part: the requirement of transmission performance and testing method) ", QB2506-2006 " optical resin spectacles lens " regulation to be detected, result is as follows:
Measure the item | Measured value |
Safety performance | 89.5 gram/127cm |
Specific refractory power | 1.555 |
Abbe number | 43 |
Anti-ultraviolet property | 400nm |
The visible transmission ratio | 99.0% |
embodiment 2 composite formulas and eyeglass preparation technology
(1) fill a prescription 2:
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 250 grams
Hexamethylene vulcabond 200 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 550 grams
Dichloride dibutyl tin 1.0 grams
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 12 grams
Zelecun 0.8 gram
Solvent violet dyestuff 0.3 gram
(2) preparation technology:
Monomer is added in the reactor of sealing after 2 amount weighings by formula, use dry nitrogen replacement to fall air.Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Reactions steps | Temperature of reaction | Reaction times |
1) | Room temperature---35 ℃ | 0.5 hour |
2) | 35℃ | 1 hour |
3) | 35℃---40℃ | 2 hours |
4) | 40℃---60℃ | 3 hours |
5) | 60℃ | 4 hours |
6) | 60℃---120℃ | 7 hours |
7) | 120℃ | 2 hours |
8) | 120℃---70℃ | 1 hour |
Then remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 115 degrees centigrade is processed.
Prepared eyeglass, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
(3) performance test
Adopt the method for ISO8980.3-2004 " burr glasses lens third part: the requirement of transmission performance and testing method ", QB2506-2006 " optical resin spectacles lens " regulation to be detected, result is as follows:
Measure the item | Measured value |
Safety performance | 73.3 gram/127cm |
Specific refractory power | 1.557 |
Abbe number | 42 |
Anti-ultraviolet property | 400nm |
The visible transmission ratio | 99.3% |
embodiment 3 composite formulas and eyeglass preparation technology
(1) fill a prescription 3:
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 160 grams
Hexamethylene vulcabond 250 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 590 grams
Dichloride dibutyl tin 1.7 grams
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 18 grams
Zelecun 1.1 grams
Solvent violet dyestuff 0.7 gram
(2) preparation technology:
Monomer is added in the reactor of sealing after 3 weighings by formula, use dry nitrogen replacement to fall air.Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Reactions steps | Temperature of reaction | Reaction times |
1) | Room temperature---35 ℃ | 0.5 hour |
2) | 35℃ | 1 hour |
3) | 35℃---40℃ | 2 hours |
4) | 40℃---60℃ | 3 hours |
5) | 60℃ | 4 hours |
6) | 60℃---120℃ | 7 hours |
7) | 120℃ | 2 hours |
8) | 120℃---70℃ | 1 hour |
Then, remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 125 degrees centigrade is processed.
Prepared eyeglass, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
(3) performance test
Adopt the method for ISO8980.3-2004 " burr glasses lens third part: the requirement of transmission performance and testing method ", QB2506-2006 " optical resin spectacles lens " regulation to be detected, result is as follows:
Measure the item | Measured value |
Safety performance | 95.2 gram/127cm |
Specific refractory power | 1.559 |
Abbe number | 42 |
Anti-ultraviolet property | 400nm |
The visible transmission ratio | 99.2% |
embodiment 4 composite formulas and eyeglass preparation technology
(1) join: 4:
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 300 grams
Hexamethylene vulcabond 110 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 590 grams
Dichloride dibutyl tin 0.7 gram
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 18 grams
Zelecun 1.1 grams
Solvent violet dyestuff 0.7 gram
(2) preparation technology:
Monomer is added in the reactor of sealing after 4 weighings by formula, use dry nitrogen replacement to fall air.Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Reactions steps | Temperature of reaction | Reaction times |
1) | Room temperature---35 ℃ | 0.5 hour |
2) | 35℃ | 1 hour |
3) | 35℃---40℃ | 2 hours |
4) | 40℃---60℃ | 3 hours |
5) | 60℃ | 4 hours |
6) | 60℃---120℃ | 7 hours |
7) | 120℃ | 2 hours |
8) | 120℃---70℃ | 1 hour |
Then remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 125 degrees centigrade is processed.
Prepared eyeglass, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
(3) performance test
Adopt the method for ISO8980.3-2004 " burr glasses lens third part: the requirement of transmission performance and testing method ", QB2506-2006 " optical resin spectacles lens " regulation to be detected, result is as follows:
Measure the item | Measured value |
Safety performance | 40.1 gram/127cm |
Specific refractory power | 1.559 |
Abbe number | 41 |
Anti-ultraviolet property | 400nm |
The visible transmission ratio | 98.8% |
embodiment 5 composite formulas and eyeglass preparation technology
(1) fill a prescription 5:
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 200 grams
Hexamethylene vulcabond 300 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 500 grams
Dichloride dibutyl tin 0.7 gram
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 18 grams
Zelecun 1.1 grams
Solvent violet dyestuff 0.7 gram
(2) preparation technology:
Monomer is added in the reactor of sealing after 5 weighings by formula, use dry nitrogen replacement to fall air.Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
Reactions steps | Temperature of reaction | Reaction times |
1) | Room temperature---35 ℃ | 0.5 hour |
2) | 35℃ | 1 hour |
3) | 35℃---40℃ | 2 hours |
4) | 40℃---60℃ | 3 hours |
5) | 60℃ | 4 hours |
6) | 60℃---120℃ | 7 hours |
7) | 120℃ | 2 hours |
8) | 120℃---70℃ | 1 hour |
Then remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 125 degrees centigrade is processed.
Prepared eyeglass, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
(3) performance test
Adopt the method for ISO8980.3-2004 " burr glasses lens third part: the requirement of transmission performance and testing method ", QB2506-2006 " optical resin spectacles lens " regulation to be detected, result is as follows:
Measure the item | Measured value |
Safety performance | 20 grams/127cm |
Specific refractory power | 1.552 |
Abbe number | 44 |
Anti-ultraviolet property | 400nm |
The visible transmission ratio | 99.0% |
Should be noted that; the foregoing is only preferred embodiment of the present invention; be not limited to scope of the present invention, all any modifications of making within the spirit and principles in the present invention, the replacement be equal to and improvement etc., within all should being included in protection scope of the present invention.
Claims (1)
1. one kind is utilized following composition of filling a prescription to prepare the method for the eyeglass that security is good,
3-isocyanic ester methylene-3,5,5-3-methyl cyclohexanol based isocyanate 250 grams
Hexamethylene vulcabond 200 grams
Four (3-thiohydracrylic acid) pentaerythritol ester, 550 grams
Dichloride dibutyl tin 1.0 grams
The tertiary octyl phenyl of 2-(2'-hydroxyl-5'-) benzotriazole 12 grams
Zelecun 0.8 gram
Solvent violet dyestuff 0.3 gram
It is characterized in that, the method is:
Monomer is added in the reactor of sealing after by the formula ratio weighing, use dry nitrogen replacement to fall air; Then mix and blend after 1 ~ 2 hour at room temperature, decompression is filled in the glass mold fixing with adhesive tape after stirring after 30 minutes above-mentioned composition being filtered with 1 micron filter, and the mould that filling is good is put into baking oven and carried out polyreaction by following heating schedule:
℃ 0.5 hour, room temperature-35
35 ℃--35 ℃ 1 hour
35 ℃--40 ℃ 2 hours
40 ℃--60 ℃ 3 hours
60 ℃--60 ℃ 4 hours
60 ℃--120 ℃ 7 hours
120 ℃ 2 hours
120 ℃--70 ℃ 1 hour
Then remove glass mold in the time of 70 ℃, the resulting eyeglass stress-removal of being annealed at the temperature of 115 degrees centigrade is processed;
The eyeglass of preparation, through the silane coupling agent that contains hydrolysis on cleaning surface dip-coating, coating the curing hard membrane layer that adds that obtains 2.0 microns of thickness of silicon sol dispersion liquid, the use vacuum vapour deposition makes lens surface obtain the antireflection rete that contains silicon-dioxide and zirconia film.
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CN105022105A (en) * | 2015-08-20 | 2015-11-04 | 万新光学集团有限公司 | Method for manufacturing silicon nitride nanometer super-hard film layer resin lens |
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WO2010095837A2 (en) * | 2009-02-17 | 2010-08-26 | 주식회사 케이오씨솔루션 | Resin composition for a high refractive index optical lens having superior impact resistance, high refractive index optical lens using same, and method for producing same |
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