Continuous preparation method of alicyclic epoxy compound

A technology of cycloaliphatic epoxy and compounds, applied in chemical instruments and methods, chemical/physical/physical chemical processes, chemical/physical/physical chemical reactors, etc. Problems such as complex process, high reaction conversion rate and yield, low process risk, and uniformity

Active Publication Date: 2021-09-28
CHANGZHOU TRONLY ADVANCED ELECTRONICS MATERIALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a continuous preparation method of cycloaliphatic epoxy compounds to solve the probl

Method used

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  • Continuous preparation method of alicyclic epoxy compound
  • Continuous preparation method of alicyclic epoxy compound
  • Continuous preparation method of alicyclic epoxy compound

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[0023] As described in the background art section, the prior art has the problems of low oxidation activity of oxidizing agents, complicated operation process and low conversion rate of conventional static microtubular reactors. In order to solve this problem, the present invention provides a continuous preparation method of cycloaliphatic epoxy compounds, which includes the following steps: S1, passing alicyclic olefin and hydrogen peroxide aqueous solution continuously into a microemulsifier for emulsification to form an emulsion , wherein the concentration of hydrogen peroxide aqueous solution ≥ 8wt%; S2, the emulsion is continuously passed into the microreactor for oxidation reaction to obtain the crude mother liquor; S3, the crude mother liquor is purified to obtain the alicyclic epoxy compound.

[0024] The present invention adopts a dynamic microtubular reactor, ensures the homogeneity of the reaction system through the combination of a microemulsifier and a microreactor...

Embodiment 1

[0047] Such as figure 1 As shown, in the alicyclic olefin feeding tank 10, 4-(2-cyclohex-3-en-1-ylpropyl-2-yl) cyclohexene 2040g, catalyst cetylpyridinium phosphotungstic acid quaternary ammonium salt 100g, 1200g of chloroform, and 150g of sodium dihydrogen phosphate are passed into the microemulsifier 50 with a flow rate of 10L / h by the first metering pump 20 under stirring conditions, and during this period, when it reaches the microemulsifier 50 through pipeline heating The temperature reaches 60-70°C. Simultaneously, the hydrogen peroxide aqueous solution feed tank 30 that 27% hydrogen peroxide aqueous solution 2510g is housed passes in the microemulsifier 50 with the flow rate of 5.8L / h through the second metering pump 40, and during this period, when it reaches the microemulsifier 50 by pipeline heating The temperature reaches 30-40°C. During the continuous feeding process, the double bond in the alicyclic olefin and the H in the hydrogen peroxide aqueous solution 2 o...

Embodiment 2

[0049] The difference with Example 1 is that the flow rate of the hydrogen peroxide aqueous solution is controlled to be 4.3L / h, and in the continuous feeding process, the double bond in the alicyclic olefin and the H in the hydrogen peroxide aqueous solution 2 o 2 The molar ratio is 1:0.7, and the mother liquor flowing out from the upper part enters the microreactor at a flow rate of 14.3L / h. Final product viscosity 90cps / 25°C, epoxy equivalent 256g / mol; olefin conversion 70%, 4-(2-cyclohex-3-en-1-ylpropyl-2-yl)epoxycyclohexane 35% , 4-(2-cyclohex-3-epoxy-1-ylpropyl-2-yl)epoxycyclohexane 33%, total yield 87%.

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Abstract

The invention provides a continuous preparation method of an alicyclic epoxy compound. The preparation method comprises the following steps: S1, continuously introducing alicyclic olefin and a hydrogen peroxide aqueous solution into a micro-emulsifier for emulsification to form an emulsion, the concentration of the hydrogen peroxide aqueous solution being greater than or equal to 8wt%; s2, continuously introducing the emulsified liquid into a microreactor for oxidation reaction to obtain a crude product mother solution; and S3, purifying the crude product mother liquor to obtain the alicyclic epoxy compound. According to the preparation method, the dynamic micro-channel reactor is adopted, the homogeneity of the reaction system is ensured through the combination of the micro-emulsifier and the micro-reactor, and the problem of poor mixing effect is avoided, so that relatively high reaction conversion rate and yield of alicyclic epoxy compound preparation can be realized by adopting the low-concentration hydrogen peroxide aqueous solution as the oxidizing agent. Besides, a continuous operation process is adopted, so that the process is small in danger, safe and controllable.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a continuous preparation method of alicyclic epoxy compounds. Background technique [0002] Alicyclic epoxy compounds play an important role in cationic curing systems, and their epoxy groups do not come from epichlorohydrin, but from olefins through oxidation, which determines that their properties are different from those of bisphenol A epoxy resins or Glycidyl ether, the epoxy group of the alicyclic epoxy compound is directly connected to the alicyclic ring, which can form a tight rigid molecular structure, and the crosslinking density increases after curing, so the heat distortion temperature is high, the curing shrinkage is small, and the stretch It has high strength, and because no chlorine-containing structure is used in the synthesis process, it has good dielectric properties and its weather resistance is also outstanding. Therefore, whether it is in the field of coating...

Claims

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Application Information

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IPC IPC(8): C07D301/12C07D303/04B01J19/00
CPCC07D301/12C07D303/04B01J19/0093
Inventor 钱晓春翁云峰
Owner CHANGZHOU TRONLY ADVANCED ELECTRONICS MATERIALS CO LTD
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