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1,3,5-Tricyclothiopropylmercaptomethylbenzene compound and preparation method thereof

A technology of thiopropyl mercaptomethylbenzene and oxypropyl mercaptomethyl benzene is applied in the field of preparation of high transmittance and high refractive index episulfide resin monomers, and can solve the problem of easy yellowing of products, insufficient product purity, Reduced optical performance, etc.

Active Publication Date: 2020-07-07
JIANGSU SHIKEXINCAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional preparation of ring sulfur from epoxy is carried out by oxygen-sulfur exchange on the ring, but due to the long reaction time, the product is easy to yellow, and there are many by-products, or the reaction temperature is too high, which often leads to the formation of by-products, leading to The purity of the product is not enough, which reduces the optical performance

Method used

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  • 1,3,5-Tricyclothiopropylmercaptomethylbenzene compound and preparation method thereof
  • 1,3,5-Tricyclothiopropylmercaptomethylbenzene compound and preparation method thereof
  • 1,3,5-Tricyclothiopropylmercaptomethylbenzene compound and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene and resin lenses.

[0030] (1) Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene: add 50 g of 1,3,5-triepoxypropyl mercaptomethylbenzene, 160 g of potassium thiocyanide, and 400 g of ethanol in a glass container , 400 g of dichloromethane, and 250 g of water were stirred and dissolved at 56° C., and the stirring was continued for about 5 hours. Then extracted with chloroform 800g×3, and the collected organic phase was washed with water three times, dried over anhydrous sodium sulfate, filtered and rotary evaporated to obtain light yellow 1,3,5-tricyclothiopropylmercaptomethylbenzene liquid. Add 1.8g of chloroform and 4.0g of attapulgite adsorbent, heat up to 45°C, stir and mix for 15 minutes, let stand for 2.5 hours, filter and remove the lower layer of attapulgite adsorbent and chloroform, and finally obtain 43.2g of colorless and transparent 1,3,5-Tricyclothiopropylmercaptomethylbe...

Embodiment 2

[0036] Example 2: Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene and resin lenses

[0037] (1) Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene: add 50 g of 1,3,5-triepoxypropyl mercaptomethylbenzene, 110 g of potassium thiocyanide, and 300 g of ethanol in a glass container , 300 g of dichloromethane, and 160 g of water were stirred and dissolved at 56° C., and the stirring was continued for about 5 hours. Then extract with chloroform 650g×3, wash the collected organic phase 3 times with water, dry over anhydrous sodium sulfate, filter and rotary evaporate to obtain light yellow 1,3,5-tricyclothiopropylmercaptomethylbenzene liquid, add 1.5g of chloroform, 2.5g of attapulgite adsorbent, heated up to 45°C, stirred and mixed for 15 minutes, left to stand for 2.5 hours, filtered to remove the attapulgite adsorbent and chloroform in the lower layer, and finally obtained 41.5g of colorless and transparent 1 , 3,5-Tricyclothiopropylmercaptomethylbenzene...

Embodiment 3

[0040] Example 3: Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene and resin lenses

[0041] (1) Preparation of 1,3,5-tricyclic thiopropylmercaptomethylbenzene: add 50 g of 1,3,5-triepoxypropyl mercaptomethylbenzene, 240 g of sodium thiocyanide, and 460 g of methanol in a glass container , dichloromethane 460g, water 280g, stir and dissolve at 58°C, continue to stir for about 5 hours, then extract with chloroform 900g×3, wash the collected organic phase with water for 3 times, dry over anhydrous sodium sulfate, and filter After rotary evaporation to obtain a light yellow 1,3,5-tricyclic thiopropylmercaptomethylbenzene liquid, add 2.0g of chloroform and 4.0g of attapulgite adsorbent, heat up to 50°C, stir and mix for 15 minutes, then let it stand After 2.5 hours, the attapulgite adsorbent and chloroform in the lower layer were removed by filtration, and finally 44.0 g of colorless and transparent 1,3,5-tricyclic thiopropylmercaptomethylbenzene was obtained.

[00...

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Abstract

The invention relates to a 1,3-5-tricyclic sulfur propyl mercaptomethyl benzene compound and a preparing method thereof. The preparing method comprises the steps that tri-epoxy propyl mercaptomethyl benzene reacts with rhodanide, an ethanol, dichloromethane and water mixed solvent serves as a reaction solvent, trichloromethane is used for extraction, attapulgite is used for adsorbing impurities, and high-purity colorless 1,3-5-tricyclic sulfur propyl mercaptomethyl benzene is obtained. The 1,3-5-tricyclic sulfur propyl mercaptomethyl benzene compound prepared with the method is high in purity and refractive index and also has the advantages of being high in transmittance and the like, wherein the light transmittance is higher than or equal to 89%, the refractive index is higher than or equal to 1.65, and the yellow index is smaller than or equal to 1.

Description

technical field [0001] The invention relates to a preparation method of a high transmittance and high refractive index episulfide resin monomer, in particular to a preparation method of 1,3,5-tricyclic thiopropylmercaptomethylbenzene. Background technique [0002] The introduction of sulfur into the polymer can increase its refractive index. Compared with other groups, it is the most effective way. At the same time, it has the advantages of small dispersion and good environmental stability. Sulfur element usually exists in the form of sulfide, thioester, sulfone group, etc. in the polymer, and also exists in the form of episulfide and polymerized with episulfide group. This form can significantly increase the sulfur content of the polymer. of. The existence of the form of episulfide not only further increases the sulfur content in the polymer, but also can be cross-linked and polymerized into a thermosetting resin under the action of a curing agent, which has the advantages...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D331/02G02B1/04C08G75/08
CPCC07D331/02C08G75/08G02B1/041
Inventor 王明华李国栋张宗弢潘敏郑永华薛晓花赵东兴刘洋司云凤
Owner JIANGSU SHIKEXINCAI CO LTD
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