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A kind of polyurethane type high refraction sulfur-containing optical resin monomer and preparation method thereof

An optical resin, high refraction technology, used in 2 fields, can solve the problems of inability to use optical materials, and achieve the effects of high purity, low yellowness index, and high light transmittance

Active Publication Date: 2017-12-12
JIANGSU SHIKEXINCAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such materials have strong optical absorption coupling in the visible light region, and cannot be used as optical materials.

Method used

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  • A kind of polyurethane type high refraction sulfur-containing optical resin monomer and preparation method thereof
  • A kind of polyurethane type high refraction sulfur-containing optical resin monomer and preparation method thereof
  • A kind of polyurethane type high refraction sulfur-containing optical resin monomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Embodiment 1: prepare 2,3-dimercaptoethylthiopropanethiol compound and polyurethane lens

[0037] (1) Preparation of 2,3-dimercaptoethylthiopropanethiol compound:

[0038] ① Mix and stir 100g of mercaptoethanol (ME) and 15g of 35wt% sodium hydroxide (NaOH) aqueous solution, control the temperature of the water bath at 46°C, add 70g of epichlorohydrin slowly within 30min, keep warm at 46°C for 100min, and the sodium salt precipitates . Then add 30g of 35wt% NaOH solution dropwise, after the color of the system turns from reddish to colorless, stir for 10 minutes, slowly add 124g of concentrated hydrochloric acid, evaporate water and by-products under reduced pressure, and then filter to remove sodium chloride to obtain sulfur generation of polyols.

[0039] ② Mix and stir 30g of thiopolyol, 34g of thiourea and 49g of concentrated hydrochloric acid, raise the temperature to 110°C, reflux for 6 hours, and stop heating. After the system cools down to 65°C, keep it warm, ...

Embodiment 2

[0047] Embodiment 2: prepare 2,3-dimercaptoethylthiopropanethiol compound and polyurethane lens

[0048] (1) Preparation of 2,3-dimercaptoethylthiopropanethiol compound:

[0049] ①Mix and stir 100g of mercaptoethanol (ME) and 12g of 35wt% sodium hydroxide (NaOH) aqueous solution, control the temperature of the water bath at 46°C, add 62g of epichlorohydrin slowly within 30min, keep warm at 46°C for 120min, and the sodium salt precipitates . Then add 24g of 35wt% NaOH solution dropwise, after the color of the system turns from reddish to colorless, stir for 10 minutes, slowly add 118g of concentrated hydrochloric acid, evaporate water and by-products under reduced pressure, and filter to remove sodium chloride to obtain sulfur generation of polyols.

[0050] ② Mix and stir 30g of thiopolyol, 30g of thiourea and 36g of concentrated hydrochloric acid, raise the temperature to 110°C, reflux for 5 hours, and stop heating. After the system cools down to 65°C, keep it warm, and ke...

Embodiment 3

[0053] Embodiment 3: prepare 2,3-dimercaptoethylthiopropanethiol compound and polyurethane lens

[0054] (1) Preparation of 2,3-dimercaptoethylthiopropanethiol compound:

[0055] ① Mix and stir 100g of mercaptoethanol (ME) and 20g of 35wt% sodium hydroxide (NaOH) aqueous solution, control the temperature of the water bath at 46°C, add 85g of epichlorohydrin slowly within 30min, keep warm at 46°C for 110min, and the sodium salt precipitates . Then add 40g of 35wt% NaOH solution dropwise, after the color of the system turns from reddish to colorless, stir for 10 minutes, slowly add 130g of concentrated hydrochloric acid, evaporate water and by-products under reduced pressure, and then filter to remove sodium chloride to obtain sulfur generation of polyols.

[0056] ② Mix and stir 30g of thiopolyol, 45g of thiourea and 59g of concentrated hydrochloric acid, raise the temperature to 110°C, reflux for 8 hours, and stop heating. After the system cools down to 70°C, keep it warm, ...

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Abstract

The invention relates to a polyurethane type high-refraction optical resin monomer containing sulfur and a preparation method of the polyurethane type high-refraction optical resin monomer. The preparation method includes: using mercaptoethanol as the raw material to synthesize a 2, 3-dimercapto ethyl sulfo-propanethiol monomer through sulfo-polyol and sulfo-polymercaptan, and allowing the 2, 3-dimercapto ethyl sulfo-propanethiol monomer to have a polymerization addition reaction with isocyanate to prepare an optical resin lens with high refraction rate and high light transmittance.\The polyurethane type optical resin monomer prepared by the method is high in purity, and the monomer and the lens are high in refraction rate, high in light transmittance, and the like. The light transmittance of the monomer is not smaller than 89%, the refraction rate of the monomer is not smaller than 1.66, the abbe number of the monomer is not smaller than 31, and the yellow index of the monomer is not larger than 0.8. The light transmittance of the lens is not smaller than 90%, the refraction rate of the lens is not smaller than 1.67, the yellow index of the lens is not larger than 1.55, and the surface hardness of the lens is 2H.

Description

technical field [0001] The invention relates to a high-refraction sulfur-containing optical resin monomer and a preparation method thereof, in particular to a preparation method of 2,3-dimercaptoethylthiopropanethiol (BES). Background technique [0002] The refractive index is directly proportional to the molar refraction and inversely proportional to the molecular volume, and the molar refraction is directly proportional to the polarizability of the medium. Therefore, in order to increase the refractive index of the resin, it is mainly by introducing groups with higher molar refraction and smaller molecular volume into the molecular structure of the polymer. From the research status at home and abroad, there are mainly the following methods: Introduce aromatic compounds, condensed ring compounds or aliphatic polycyclic compounds to increase the refractive index; introduce halogen elements (except F) or heteroelements such as sulfur, nitrogen, phosphorus to increase the refr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C321/14C07C319/20C08G18/38G02B1/04
CPCC07C319/14C07C319/20C07C321/14C08G18/3876G02B1/04C07C323/12
Inventor 王明华纪立军郑莹司云凤范为正徐静涛张鹤军张安震薛晓花郑永华
Owner JIANGSU SHIKEXINCAI CO LTD
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