Preparation method of epoxy compound

A technology for epoxy compounds and hydrogen sulfide, which is applied in chemical instruments and methods, chemical/physical processes, organic compounds/hydrides/coordination complex catalysts, etc. and other problems, to achieve the effect of less investment in equipment, low cost of raw materials, and simple operation

Active Publication Date: 2020-09-11
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although the existing reported methods all synthesize higher-quality structural compounds shown in formula (I), the amount of solvent is large, and it is not easy to recycle, and a large amount of waste water will be generated, the pollution of three wastes is large, and the production cost is high.

Method used

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  • Preparation method of epoxy compound
  • Preparation method of epoxy compound
  • Preparation method of epoxy compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A kind of preparation method of episulfide compound, its specific method is:

[0036] 1) Add 56.1g of quaternary ammonium strong base anion exchange resin catalyst, 561g of methanol, and 187g of epichlorohydrin into a 1000mL four-neck bottle, stir, cool down to 5°C, and then feed 1.05 moles of hydrogen sulfide gas into the mixed solution, and feed the gas The speed was 1.0L / h, and reacted for 3 hours after passing through the hydrogen sulfide. At this time, there was no raw material left, and it was filtered. The filtrate was distilled off the solvent under reduced pressure, and the intermediate A was obtained after spin-drying methanol. The content was 98.95%, and the yield 99.23%; catalyst resin and solvent can continue to be used as the next batch of reactions;

[0037] 2) Add 549.29g of guanidine-based resin catalyst, 549.29g of tetrahydrofuran, and 219.72g of intermediate A into a 1000mL four-neck flask, heat up to 40°C, and react for two hours. When the mass fract...

Embodiment 2

[0039] A kind of preparation method of episulfide compound, its specific method is:

[0040] 1) In a 1000mL four-necked bottle, add quaternary ammonium strong base anion exchange resin catalyst (this catalyst is the seventh time application of the quaternary ammonium strong base anion exchange resin in Example 1) 56.1g, methanol 561g, epichlorohydrin 187g, stir, cool to 2 ℃, then feed 1.05 moles of hydrogen sulfide gas into the reaction solution, the speed of feeding the gas is 2.2L / h, and react for 3.5 hours after the hydrogen sulfide is passed through. Solvent, obtain intermediate A after spin-drying methanol, its content is 96.52%, yield 98.13%; Catalyst resin and solvent can continue to be used as next batch of reaction;

[0041] 2) In a 1000mL four-necked bottle, add guanidine-based resin catalyst (this catalyst is the third application of guanidine-based resin in Example 1) 556.63g, ethylene glycol phenyl ether 556.63g, intermediate A 222.65g, and heat up to 60 DEG C, r...

Embodiment 3

[0043] A kind of preparation method of episulfide compound, its specific method is:

[0044]1) Add 56.1g of quaternary ammonium strong base anion exchange resin catalyst, 561g of methanol, and 187g of epichlorohydrin into a 1000mL four-necked bottle, stir, heat up to 8°C, then feed 1.05 moles of hydrogen sulfide gas into the reaction solution, and feed the The speed was 5L / h, and reacted for 4 hours after the hydrogen sulfide was passed through. At this time, there was no raw material left, and it was filtered. The filtrate was distilled off the solvent under reduced pressure, and the intermediate A was obtained after spin-drying methanol. %; Catalyst resin and solvent can continue to be used as next batch of reaction simultaneously;

[0045] 2) Add 548.28g of guanidinium resin catalyst, 548.28g of ethylene glycol phenyl ether, and 219.31g of intermediate A into a 1000mL four-neck flask, heat up to 60°C, and react for 3 hours, and react when the mass fraction of intermediate A...

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Abstract

The invention belongs to the technical field of organic synthesis. The invention particularly relates to a preparation method of an epoxy compound. The specific preparation method comprises the following steps: with epihalohydrin as a raw material and H2S as a sulfo-hybridization reagent, performing a catalytic reaction under a resin catalyst to prepare the epoxy compound; according to the preparation method, the reaction conditions are mild, the operation is simple, the equipment investment is low and the raw material cost is low. The method is free of waste gas, liquid and solids, wherein the adopted solvent is a single solvent and is convenient to recycle, and the catalyst resin can be recycled, so that the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of epoxy compounds. Background technique [0002] The higher the refractive index, the thinner the lens, that is, the center of the lens has the same thickness, the same degree and the same material, and the edge of the lens with a high refractive index is thinner than that of a lens with a low refractive index. The pursuit of high refractive index has become the development trend of the lens industry. In order to increase the refractive index, introducing sulfur into the polymer is the most effective way to increase the refractive index. At the same time, the material has small dispersion and good environmental stability. In recent years, there are relatively many reports on increasing the refractive index of optical resins by introducing sulfur into polymers. Sulfur in polymers is usually introduced in the form of thioether bonds, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/34C07D301/26B01J31/08B01J38/64
CPCC07D303/34C07D301/26B01J31/08B01J38/64Y02P20/584
Inventor 张金国张建林丁宗旺曹帅易先君曹飞羽侯小敏刘洋
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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