CN101614831B - High refractivity resin lens and preparation method thereof - Google Patents
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Abstract
The invention discloses a high refractivity resin lens and a preparation method thereof; the preparation method comprises the following steps: mixing one or more of sulfur-containing monomers with one or more of polyisocyanates or isothiocyanate compound in a molar ratio of 0.8-1.3:1 evenly, then adding phosphate internal releasing agent accounting for 0.05-2% of the total mass of the above mixture and organo-tin catalyst accounting for 0.005-0.1% of the total mass of the above mixture, then adding light stabilizer, ultraviolet absorbent and antioxidant according to the standards and demands of resin lens synthesis and obtaining the lens by polymerization. The refractivity nD of the lens prepared by the method of the invention can reach 1.6725, the comprehensive performance is increased and the lens can be widely used as the lens of the telescope, the sighting telescope, the magnifier and the camera, thus expanding the application range of the resin lens.
Description
Technical field
The invention belongs to the organic chemistry synthesis technical field, relate to high refractivity resin lens and preparation method thereof.
Background technology
The material that current eyeglass is used is except adopting unorganic glass, and employing has the research and development constantly development of the synthetic resin of superior optical characteristics as lens materials, and the trend that progressively replaces the conventional lenses material is arranged.Resin lens is compared with the unorganic glass eyeglass, and its feature is: in light weight, transparency is high, lens dimension is big, shock resistance, easily machine-shaping, can dye etc.Resin sheet is in preferential status in the glasses market competition.It is reported that the optics resin lens accounted for 65% in the U.S. in 1988, Japan accounts for 55%.Recently in 3,200 ten thousand people of Japanese wearing spectacles, have 85%～90% approximately, select resin lens for use.The synthetic resin optical mirror slip is to adopt the polyene propyl group diglycol carbonates that nineteen forty-two is developed to by U.S. PPG company at first, and this is a kind of heat cured synthetic resin, and commodity are called CR-39, have more excellent cutting and grinding, thermotolerance, resistance to chemical reagents.Proportion is 1.32, and lighter about half than the proportion 2.58 of inorganic optical glass, dyeing is also easier.CR-39 is succeeded in developing by U.S. Colombia research department, so have another name called Colombia's resin, occupies leading position in resin lens market.But widely used in the market optical resin material such as polymethylmethacrylate (PMMA), CR-39 etc. have lower refractive index (n
D＜1.50), traditional the highest PS of optical resin refractive index also only reaches n
D=1.590, and combination property is not really desirable, has so just limited the range of application of material.And according to the requirement of glasses market popularity style, lens materials also requires eyeglass is made not only light but also thin except should having preferably optical property, and this has become the main direction in the current resin lens research and development.Therefore, synthetic new varieties high-performance transparent resin becomes the inexorable trend of optical plastic development, and the research of preparation high refractive index, high-performance transparent optical resin has become focus.
Summary of the invention
The object of the present invention is to provide high refractivity resin lens and preparation method thereof, mainly make by designing synthetic or selecting corresponding high sulfur content monomer and polyisocyanates or isothiocyanate compound, solve the existing problem of background technology by the synthetic high refractivity resin lens of copolymerization.
The concrete scheme that realizes the object of the invention is:
A kind of high refractivity resin lens, characteristics are: with one or more sulfur-bearing monomers and one or more polyisocyanates or isothiocyanate compound is that 0.8～1.3: 1 ratio mixes in molar ratio, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for aforementioned potpourri gross mass 0.05～2%, the organic tin catalyzer that accounts for aforementioned potpourri gross mass 0.005～0.1% then, standard-required according to synthetic resin lens adds light stabilizer, ultraviolet absorber, antioxidant again, gets the resin lens of high index of refraction through polymerization;
Described sulfur-bearing monomer is the compound of high sulfur content, wherein contain two sulfydryls or hydroxy functional group or hydroxyl compound of a sulfydryl at least, these compounds comprise sulfo-glycerine (SR1), benzene dimethanethiol (SR2), 2,3-dimercapto ethylenebis dithiocarbamate propanethiol (SR3), 2,3-dimercapto propyl dithiocarbamate propanethiol (SR4), 3-mercaptoethyl sulfo-dimercaptopropane (SR5), Ji Wusi mercaptan (SR6), mercaptoacetic acid pentaerythritol ester (SR7), 3,3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide (SR8) and 1,3-two sulfo-propyl alcohol (SR9);
Described polyisocyanates or isothiocyanate compound, wherein contain two or more the isocyanate functional group or the compound of isothiocyanates functional group at least, these compounds comprise toluene diisocyanate (TDI), toluene diisocyanate (TSTI), hexamethylene diisocyanate (HDI), own diisothio-cyanate (HDTI), dicyclohexyl methyl hydride diisocyanate (HMDI), phenylmethane diisocyanate (MDI), phenylmethane diisothio-cyanate (MDTI), Xylene Diisocyanate (XDI), dimethylbenzene diisothio-cyanate (XDTI), isophorone diisocyanate (IPDI) and isophorone diisothio-cyanate (IPDTI).
A kind of preparation method of above-mentioned resin lens, characteristics are: synthetic earlier or selection high sulfur content monomer, then this monomer and one or more polyisocyanates or isothiocyanate compound are mixed in proportion, in the presence of catalyzer, release agent, antioxidant, ultraviolet absorber, the injection molding copolymerization is synthetic, the concrete operations step:
The preparation of first step high sulfur content monomer
Synthesizing of sulfo-glycerine (SR1)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, add 1,2 of 0.05mol, the concentrated hydrochloric acid of 3-trichloropropane, 0.2～0.4mol thiocarbamide and 0.2～0.5mol, carry out reflux and stir 24h, behind the cool to room temperature, add the ammoniacal liquor of 0.3～0.6mol then, slowly be warmed up to 60 ℃, after carrying out heated and stirred 5h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets product SR1 after the distillation;
Synthesizing of benzene dimethanethiol (SR2)
The concentrated hydrochloric acid that in having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, adds benzene dimethanol, 0.1～0.3mol thiocarbamide and the 0.1～0.4mol of 0.05mol, carry out reflux and stir 30h, behind the cool to room temperature, add the ammoniacal liquor of 0.1～0.4mol then, slowly be warmed up to 65 ℃, after carrying out heated and stirred 4h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets product SR2 after the distillation;
2,3-dimercapto propyl dithiocarbamate propanethiol (SR4) synthetic
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.1mol, under 30～40 ℃ of conditions, drip the 0.005mol epichlorokydrin then, drip off the back and continue reaction 1～2h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.05～0.3mol, slowly be warmed up to 60 ℃, carry out heated and stirred 4h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR4 after the distillation;
Synthesizing of 3-mercaptoethyl sulfo-dimercaptopropane (SR5)
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.05mol, under 30～40 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 1～2h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.05～0.3mol, slowly be warmed up to 65 ℃, carry out heated and stirred 5h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR5 after the distillation;
Synthesizing of mercaptoacetic acid pentaerythritol ester (SR7)
The pentaerythrite and the 20mL DMF that in having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube and tap funnel, add 0.01mol, slowly drip the sulfydryl acetyl chloride of 0.04～0.05mol, under 30～40 ℃ of conditions, continue reaction 1～2h then, then behind the cool to room temperature, carry out alkali cleaning, washing promptly gets product SR7 after the distillation;
3,3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide (SR8) synthetic
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.1g, under 30～40 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 0.5～2h, then drip 30% sodium sulfide solution 0.01mol, drip off the back and continue reaction 0.5～1h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.05～0.3mol, slowly be warmed up to 65 ℃, carry out heated and stirred 5h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR8 after the distillation;
The preparation of the second step high refractivity resin lens
With one or more potpourris in the above-mentioned monomer and one or more polyisocyanates or isothiocyanate compound is that 0.8～1.3: 1 ratio mixes in molar ratio, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for aforementioned potpourri gross mass 0.05～2% then, account for the organic tin catalyzer of aforementioned potpourri gross mass 0.005～0.1%, standard-required according to synthetic resin lens adds light stabilizer again, ultraviolet absorber, antioxidant, earlier after carrying out vacuum defoamation pre-polymerization 2～3h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 5～12h under this temperature promptly gets the resin lens of high index of refraction.
The eyeglass that the present invention makes, its refractive index reaches as high as n
D=1.6725, combination property is improved, and is widely used for making the lens on telescope, gun sight, magnifier and the camera, makes the range of application of resin lens more extensive.
Embodiment
Below will the present invention is further elaborated by specific embodiment:
Embodiment 1
Synthesizing of first step sulfo-glycerine (SR1)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, add 1,2 of 0.05mol, the concentrated hydrochloric acid of 3-trichloropropane, 0.3mol thiocarbamide and 0.35mol, carry out reflux and stir 24h, behind the cool to room temperature, add the ammoniacal liquor of 0.4mol then, slowly be warmed up to 60 ℃, after carrying out heated and stirred 5h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets product SR1 after the distillation;
The preparation of the second step high refractivity resin lens
SR1 and isocyanate compound were mixed in molar ratio=1: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for potpourri gross mass 0.5% then, account for the organic tin catalyzer of potpourri gross mass 0.05%, standard-required according to synthetic resin lens adds light stabilizer again, ultraviolet absorber, antioxidant, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 1.
Table 1
Embodiment 2
Synthesizing of first step benzene dimethanethiol (SR2)
The concentrated hydrochloric acid that in having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, adds benzene dimethanol, 0.15mol thiocarbamide and the 0.2mol of 0.05mol, carry out reflux and stir 30h, behind the cool to room temperature, add the ammoniacal liquor of 0.2mol then, slowly be warmed up to 65 ℃, after carrying out heated and stirred 4h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets product SR2 after the distillation;
The preparation of the second step high refractivity resin lens
SR2 and isocyanate compound were mixed in molar ratio=1.2: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for potpourri gross mass 0.5% then, account for the organic tin catalyzer of gross mass 0.05%, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 2.
Table 2
Embodiment 3
The first step 2,3-dimercapto propyl dithiocarbamate propanethiol (SR4)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube and tap funnel, add the mercaptoethanol of 0.01mol, the pyridine of 0.015mol, under 35 ℃ of conditions, drip the 0.005mol epichlorokydrin then, drip off the back and continue reaction 1h, the concentrated hydrochloric acid that adds 0.1mol thiocarbamide and 0.15mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.25mol, slowly be warmed up to 60 ℃, carry out heated and stirred 4h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR4 after the distillation;
The preparation of the second step high refractivity resin lens
SR4 and isocyanate compound were mixed in molar ratio=0.8: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for gross mass 0.5% then, account for the organic tin catalyzer of gross mass 0.05%, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 3.
Table 3
Embodiment 4
First step 3-mercaptoethyl sulfo-dimercaptopropane (SR5)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube and tap funnel, add the mercaptoethanol of 0.01mol, the pyridine of 0.015mol, under 30 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 1h, the concentrated hydrochloric acid that adds 0.05mol thiocarbamide and 0.05mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.2mol, slowly be warmed up to 65 ℃, carry out heated and stirred 5h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR5 after the distillation;
The preparation of the second step high refractivity resin lens
SR5 and isocyanate compound were mixed in molar ratio=1: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for gross mass 0.5% then, account for the organic tin catalyzer of gross mass 0.05%, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 4.
Table 4
Embodiment 5
First step mercaptoacetic acid pentaerythritol ester (SR7)
Having electromagnetic agitation, thermometer, the pentaerythrite and the 20mL DMF that add 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, slowly drip the sulfydryl acetyl chloride of 0.045mol, under 30 ℃ of conditions, continue reaction 2h then, behind the cool to room temperature, carry out alkali cleaning then, washing promptly gets product SR7 after the distillation;
The preparation of the second step high refractivity resin lens
SR5 and isocyanate compound were mixed in molar ratio=1: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for gross mass 0.5% then, account for the organic tin catalyzer of gross mass 0.05%, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 5.
Table 5
Embodiment 6
The first step 3,3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide (SR8) synthetic
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.012g pyridine, under 30～40 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 1h, then drip 30% sodium sulfide solution 0.01mol, drip off the back and continue reaction 1h, the concentrated hydrochloric acid that adds 0.15mol thiocarbamide and 0.15mol carries out reflux and stirs 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.2mol, slowly be warmed up to 65 ℃, carry out heated and stirred 5h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets product SR8 after the distillation;
The preparation of the second step high refractivity resin lens
SR8 and isocyanate compound were mixed in molar ratio=1: 1, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for gross mass 0.5% then, account for the organic tin catalyzer of gross mass 0.05%, earlier after carrying out vacuum defoamation pre-polymerization 2h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 10h under this temperature, promptly get high index of refraction and transparent resin lens, used isocyanate compound and corresponding refractive index see Table 6.
Table 6
Claims (2)
1. high refractivity resin lens, it is characterized in that: with one or more sulfur-bearing monomers and one or more polyisocyanates or isothiocyanate compound is that 0.8～1.3: 1 ratio mixes in molar ratio, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for aforementioned potpourri gross mass 0.05～2%, the organic tin catalyzer that accounts for aforementioned potpourri gross mass 0.005～0.1% then, standard-required according to synthetic resin lens adds light stabilizer, ultraviolet absorber, antioxidant again, gets the resin lens of high index of refraction through polymerization;
Described sulfur-bearing monomer is the compound of high sulfur content, wherein contain two sulfydryls or hydroxy functional group or hydroxy functional group of a sulfydryl at least, these compounds comprise sulfo-glycerine (SR1), benzene dimethanethiol (SR2), 2,3-dimercapto ethylenebis dithiocarbamate propanethiol (SR3), 2,3-dimercapto propyl dithiocarbamate propanethiol (SR4), 3-mercaptoethyl sulfo-dimercaptopropane (SR5), Ji Wusi mercaptan (SR6), mercaptoacetic acid pentaerythritol ester (SR7), 3,3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide (SR8) and 1,3-two sulfo-propyl alcohol (SR9);
Described polyisocyanates or isothiocyanate compound, wherein contain plural isocyanate functional group or isothiocyanates functional group, these compounds comprise toluene diisocyanate (TDI), toluene diisocyanate (TSTI), di-isocyanate (HDI), own diisothio-cyanate (HDTI), dicyclohexyl methyl hydride diisocyanate (HMDI), phenylmethane diisocyanate (MDI), phenylmethane diisothio-cyanate (MDTI), Xylene Diisocyanate (XDI), dimethylbenzene diisothio-cyanate (XDTI), isophorone diisocyanate (IPDI) and isophorone diisothio-cyanate (IPDTI).
2. the preparation method of the described resin lens of claim 1, it is characterized in that: synthetic earlier or selection high sulfur content monomer, then this monomer and one or more polyisocyanates or isothiocyanate compound are mixed in proportion, in the presence of catalyzer, release agent, antioxidant, ultraviolet absorber, the injection molding copolymerization is synthetic, the concrete operations step:
The preparation of first step high sulfur content monomer
Synthesizing of sulfo-glycerine (SR1)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, add 1,2 of 0.05mol, the concentrated hydrochloric acid of 3-trichloropropane, 0.2～0.4mol thiocarbamide and 0.2～0.5mol, carry out reflux and stir 24h, behind the cool to room temperature, add the ammoniacal liquor of 0.3～0.6mol then, slowly be warmed up to 60 ℃, after carrying out heated and stirred 5h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets the sulfo-glycerine after the distillation;
Synthesizing of benzene dimethanethiol (SR2)
The concentrated hydrochloric acid that in having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube, adds benzene dimethanol, 0.1～0.3mol thiocarbamide and the 0.1～0.4mol of 0.05mo1, carry out reflux and stir 30h, behind the cool to room temperature, add the ammoniacal liquor of 0.1～0.4mol then, slowly be warmed up to 65 ℃, after carrying out heated and stirred 4h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing promptly gets benzene dimethanethiol after the distillation;
2,3-dimercapto propyl dithiocarbamate propanethiol (SR4) synthetic
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mo1 in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.1mol, under 30～40 ℃ of conditions, drip the 0.005mol epichlorokydrin then, drip off the back and continue reaction 1～2h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, then behind the cool to room temperature, add the ammoniacal liquor of 0.05～0.3mol, slowly be warmed up to 60 ℃, carry out heated and stirred 4h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, washing, promptly get 2 after the distillation, 3-dimercapto propyl dithiocarbamate propanethiol;
Synthesizing of 3-mercaptoethyl sulfo-dimercaptopropane (SR5)
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.05mol, under 30～40 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 1～2h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, then behind the cool to room temperature, the ammoniacal liquor that adds 0.05～0.3mol, slowly be warmed up to 65 ℃, carry out heated and stirred 5h after, standing demix, after branch removes upper water solution, lower floor is carried out pickling, and washing promptly gets 3-mercaptoethyl sulfo-dimercaptopropane after the distillation;
Synthesizing of mercaptoacetic acid pentaerythritol ester (SR7)
In having the 100mL three-necked bottle of electromagnetic agitation, thermometer, reflux condensing tube and tap funnel, add the pentaerythrite of 0.01mol and the N of 20mL, dinethylformamide (DMF), slowly drip the sulfydryl acetyl chloride of 0.04～0.05mol, under 30～40 ℃ of conditions, continue reaction 1～2h then, then behind the cool to room temperature, carry out alkali cleaning, washing promptly gets the mercaptoacetic acid pentaerythritol ester after the distillation;
3,3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide (SR8) synthetic
Having electromagnetic agitation, thermometer, the mercaptoethanol that adds 0.01mol in the 100mL three-necked bottle of reflux condensing tube and tap funnel, 0.01 the pyridine of～0.1g, under 30～40 ℃ of conditions, drip the 0.01mol epichlorokydrin then, drip off the back and continue reaction 0.5～2h, then drip 30% sodium sulfide solution 0.01mol, drip off the back and continue reaction 0.5～1h, the concentrated hydrochloric acid that adds 0.03～0.2mol thiocarbamide and 0.05～0.2mol, carry out reflux and stir 12h, behind the cool to room temperature, add the ammoniacal liquor of 0.05～0.3mol then, slowly be warmed up to 65 ℃, after carrying out heated and stirred 5h, standing demix after branch removes upper water solution, carries out pickling to lower floor, washing, promptly get 3 after the distillation, 3 '-dimercapto ethyl-2,2 '-sulfydryl dipropyl sulfide;
The preparation of the second step high refractivity resin lens
With one or more potpourris in the above-mentioned monomer and one or more polyisocyanates or isothiocyanate compound is that 0.8～1.3: 1 ratio mixes in molar ratio, add the phosphoric acid ester inner pattern releasing agent applicable that accounts for aforementioned potpourri gross mass 0.05～2%, account for the organic tin catalyzer of aforementioned potpourri gross mass 0.005～0.1%, standard-required according to synthetic resin lens adds light stabilizer again, ultraviolet absorber, antioxidant, earlier after carrying out vacuum defoamation pre-polymerization 2～3h under 50～60 ℃, inject mould, and then at 80 ℃ of following polymerization 5h, then the programming rate with 2 ℃/min is heated to 100 ℃, polymerization 5～12h under this temperature promptly gets the resin lens of high index of refraction.
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| CN105482070B (en) * | 2015-12-08 | 2017-08-18 | 江苏乾元新材料科技有限公司 | It is a kind of to use optical resin composition with high impact resistance, heat resistance and refractive index of organic and inorganic hybridization and preparation method thereof |
| KR101835082B1 (en) * | 2017-05-16 | 2018-03-06 | 에스케이씨 주식회사 | Isocyanate composition for optical lenses and preparation method thereof |
| CN111333803B (en) * | 2018-12-19 | 2022-02-18 | 万华化学集团股份有限公司 | Optical resin composition, optical resin material and application thereof |
| CN112625217B (en) * | 2020-12-23 | 2022-07-12 | 江南大学 | Preparation method of sulfur-containing fluorene-containing structure high-refractive-index optical resin |
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