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Method for preparing tetra-sulfenyl polyhydric mercaptan and method for preparing polyurethane-based resin lens by using tetra-sulfenyl polyhydric mercaptan

A technology based on ethyl and mercapto groups, applied in the field of polyurethane-based resins, can solve the problems of low refractive index and achieve the effects of strong weather resistance, good machinability, and good impact resistance

Active Publication Date: 2012-09-19
SHANGHAI WEIXING OPTICAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ordinary polyurethane material has good impact resistance, but its refractive index is not high

Method used

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  • Method for preparing tetra-sulfenyl polyhydric mercaptan and method for preparing polyurethane-based resin lens by using tetra-sulfenyl polyhydric mercaptan
  • Method for preparing tetra-sulfenyl polyhydric mercaptan and method for preparing polyurethane-based resin lens by using tetra-sulfenyl polyhydric mercaptan

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a 500mL four-necked flask equipped with an electric stirrer, reflux condenser, thermometer and dropping funnel, add 50mL petroleum ether and 20mL 2-mercaptoethanol, cool to 0℃ with an ice water bath, and add 10mL one by one within 1 hour. A mixed solution of sulfur chloride and 50 mL of petroleum ether was then stirred for 10 hours to obtain a crude product. The obtained product was extracted and purified three times with 100 ml of water, and the organic phase was separated and dried with anhydrous calcium chloride. The petroleum ether was distilled off under reduced pressure, and the fraction at 34-38°C was collected to obtain about 25 g of colorless viscous liquid bis(22 hydroxy) ethyl tetrasulfide. Subsequently, 30.1 g of 36% hydrochloric acid and 19 g of thiourea were added to bis(22 hydroxy) ethyl tetrasulfide, stirred and heated to 110° C. for 9 hours. The mixture was cooled to room temperature, 50 ml of toluene was added thereto, and then 31 g of 25% ammonia w...

Embodiment 2

[0024] In a 500mL four-necked flask equipped with an electric stirrer, reflux condenser, thermometer and dropping funnel, add 50mL petroleum ether and 20mL 2-mercaptoglycol, cool to 0℃ with an ice water bath, and add dropwise within 1 hour A mixed solution of 10 mL of sulfur monochloride and 50 mL of petroleum ether was then stirred for 10 hours to obtain a crude product. The obtained product was extracted and purified three times with 100 ml of water, and the organic phase was separated and dried with anhydrous calcium chloride. The petroleum ether was distilled off under reduced pressure, and the fraction at 34-38°C was collected to obtain about 30 g of colorless viscous liquid bis(2222 hydroxy) ethyl tetrasulfide. Subsequently, 60.2 g of 36% hydrochloric acid and 38 g of thiourea were added to bis(2222 hydroxy) ethyl tetrasulfide, and the mixture was stirred and heated to 110° C. for 9 hours. The mixture was cooled to room temperature, 50 ml of toluene was added thereto, an...

Embodiment 3

[0027] In a 500mL four-necked flask equipped with an electric stirrer, reflux condenser, thermometer and dropping funnel, add 50mL petroleum ether and 20mL 2-mercaptopropanol, cool to 0℃ with an ice water bath, and finish the dripping within 1 hour. A mixed solution of 10 mL of sulfur monochloride and 50 mL of petroleum ether was then stirred for 10 hours to obtain a crude product. The obtained product was extracted and purified three times with 100 ml of water, and the organic phase was separated and dried with anhydrous calcium chloride. The petroleum ether was distilled off under reduced pressure, and the fraction at 34-38°C was collected to obtain about 25 g of colorless viscous liquid bis(22 hydroxy) ethyl tetrasulfide. Subsequently, 30.1 g of 36% hydrochloric acid and 19 g of thiourea were added to the bis(22 hydroxy) propyl tetrasulfide, stirred and heated to 110° C. for 9 hours. The mixture was cooled to room temperature, 50 ml of toluene was added thereto, and then 31...

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Abstract

The invention relates to a method for preparing tetra-sulfenyl polyhydric mercaptan, a method for preparing polyurethane-based resin lens by using the tetra-sulfenyl polyhydric mercaptan, a sulfur-containing polyurethane resin prepared from the tetra-sulfenyl polyhydric mercaptan and isocyanate, and a lens prepared from the resin. The method for preparing the tetra-sulfenyl polyhydric mercaptan and the method for preparing the polyurethane-based resin lens by using the tetra-sulfenyl polyhydric mercaptan have the advantages that: the resin has high refraction index, low dispersion coefficient, water white transparency, low density, no optical distortion, strong weather resisting property, capability of dyeing, good heat resistance, good impact resistance and machining performance.

Description

【Technical Field】 [0001] The invention relates to the technical field of polyurethane-based resins, in particular to a method for preparing tetrasulfide polythiol and a method for preparing polyurethane-based resin lenses using the thiol. 【Background technique】 [0002] Polymer optical materials have been widely used in optical information storage, optical communication and other fields in recent years due to their advantages of light weight, damage resistance, and easy processing and molding. They are used to make various lenses in glasses, cameras, and military products. The light guide device of the optical instrument. In the production of such devices, polymer optical materials with high refractive index and high strength are particularly important, which can further reduce the curvature and thickness of the device and reduce the weight without affecting its refractive power. [0003] Polymer optical materials have been widely used in optical information storage, optical commu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C321/14C07C319/22C08G18/38G02B1/04
Inventor 汪山献松陈国贵林晓华徐云杜丽萍
Owner SHANGHAI WEIXING OPTICAL
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