Method for producing high-quality epoxy compound

An epoxy compound, high-quality technology, applied in chemical recycling, organic chemistry, etc., can solve the problems of BCPDS content decline, poor catalyst activity, unstable intermediates, etc., achieve high promotion value, short reaction time, and stable reaction process Effect

Active Publication Date: 2017-02-15
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because in the tank reaction, the materials have different degrees of reverse mixing, the reaction time is long, and the activity of the catalyst is poor; at the same time, in the tank reactor, under the catalysis of the alkali, the intermediate in the first step is unstable and easily Occurrence of self-closed ring to generate 3-hydroxycyclopropyl sulfide or react with raw material epichlorohydrin to generate 3-chloro-2-hydroxy propyl sulfide. In addition, catalyst base reacts with hydrogen sulfide to generate alkali sulfide and bring it into the intermediate
These factors can easily lead to a decrease in BCPDS content and an increase in chroma

Method used

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  • Method for producing high-quality epoxy compound

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Experimental program
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Effect test

Embodiment 1

[0028] The fixed-bed reactor is filled with a 10% sodium hydroxide catalyst loaded with alumina, and the methanol with a content of 99% is first transported into the tubular fixed-bed reactor at a flow rate of 20 mL / min using a constant-flow pump 0, and then the methanol with a content of 99.5% epichlorohydrin was sent into the tubular fixed-bed reactor at a flow rate of 20mL / min using constant flow pump 1, and hydrogen sulfide with a content of 99.9% was sent into the tube at a flow rate of 24mL / min using booster pump 2. Type fixed-bed reactor, keep the reactor pressure at 0.1MPa, cool the tubular reactor to 0-10°C through a low-temperature circulation device to perform ring-opening substitution reaction to obtain compound 1; then add 10mol compound 1, 3780g methanol, 635g iodine , 50g of tetrabutylammonium bromide was added to the reactor for oxidation reaction, the temperature was kept at 25°C, and the reaction was carried out for 4h to obtain bis(3-chloro-2-hydroxypropyl)di...

Embodiment 2

[0030]The fixed-bed reactor is filled with a silica-loaded 10% sodium carbonate catalyst. First, methanol with a content of 99% is transported into the tubular fixed-bed reactor at a flow rate of 20 mL / min using a constant-flow pump 0, and then the methanol with a content of 99.5% epichlorohydrin was sent into the tubular fixed-bed reactor at a flow rate of 20mL / min using constant flow pump 1, and hydrogen sulfide with a content of 99.9% was sent into the tube at a flow rate of 24mL / min using booster pump 2. Type fixed-bed reactor, keep the reactor pressure at 0.1MPa, cool the tubular reactor to 0-10°C through a low-temperature circulation device to perform ring-opening substitution reaction to obtain compound 1; then add 10mol compound 1, 3780g methanol, 635g iodine , 63g of tetrabutylammonium bromide was added to the reaction kettle for oxidation reaction, and the temperature was kept at 30°C for 3 hours to obtain bis(3-chloro-2-hydroxypropyl) disulfide crude product); after ...

Embodiment 3

[0032] The fixed-bed reactor is filled with dipotassium hydrogen phosphate catalyst loaded with 10% alumina, and methanol with a content of 99% is first transported into the tubular fixed-bed reactor at a flow rate of 20 mL / min using a constant flow pump 0, and then the content is 99.5% epichlorohydrin is sent into the tubular fixed-bed reactor at a flow rate of 20mL / min using constant flow pump 1, and hydrogen sulfide with a content of 99.9% is sent into the reactor at a flow rate of 24mL / min using booster pump 2 Tubular fixed-bed reactor, keeping the reactor pressure at 0.11MPa, cooling the tubular fixed-bed reactor to 0-10°C through a low-temperature circulation device to perform ring-opening substitution reaction to obtain compound 1, and then add 10mol compound 1, 3780g methanol , 635g iodine and 37.8g tetrabutylammonium bromide were added to the reaction kettle for oxidation reaction, keeping the temperature at 20°C, and reacting for 5h to obtain bis(3-chloro-2-hydroxypro...

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Abstract

The invention provides a method for producing a high-quality epoxy compound. The method comprises the following steps: carrying out a ring opening reaction on hydrogen sulfide and chloropropylene oxide in a fixed bed reaction device in the presence of a catalyst solid alkali, and carrying out oxidation and a ring closing reaction to produce the high-quality epoxy compound. The fixed bed reaction device adopted in the invention improves the product purity to 98%, reduces the content of impurities, controls the content of monothio impurities to be 1% or less, and improves the refractive index of the product. The chroma of the product is reduced to 10-20. The method has the advantages of mild reaction conditions, easiness in filtration and recovery of the solid alkali catalyst, realization of repeated use of the catalyst after being activated, continuous production of the reaction device, and facilitation of industrial production application.

Description

technical field [0001] The invention belongs to the field of organic synthesis and epoxy compound synthesis methods, and in particular relates to a method for producing high-quality epoxy compounds. Background technique [0002] With the advancement of science, optical materials are increasingly used in technology and life. For optical materials, especially spectacle lenses, the required physical properties are low specific gravity, high transparency, low yellowness, high heat resistance, high strength, etc., and the optical properties are high refractive index and high Abbe number. Refractive index is the most basic property of optical materials, and high refractive index materials are the goal that people are increasingly pursuing today. [0003] Epoxy compounds have the characteristics of easy curing, adjustable curing conditions and good transparency, so they are widely used in the field of optical resins, such as optical devices, optical packaging and optical adhesives...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/34C07D301/26
CPCY02P20/584C07D303/34C07D301/26
Inventor 高丽娟雷雳光刘洋曹帅易先君张建林郭龙龙
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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