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Catalytic preparation method of dicyclopentadiene dioxide by quaternary ammonium heteropoly phosphato tungstate

A technology of dicyclopentadiene dioxide and phosphotungstic heteropoly acid, which is applied in the direction of organic chemistry, can solve the problems of serious equipment corrosion, complicated reaction process, poor practicability, etc., and achieves high safety, short process and easy operation. Effect

Active Publication Date: 2010-05-12
SICHUAN DONGFANG INSULATING MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, the traditional methods for preparing olefin epoxides include the chlorohydrin method and the peracid method. These methods have the disadvantages of severe equipment corrosion, complex reaction process, and the acidic ring-opening of epoxides, which may generate a series of by-products. , less practical

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0025] Preparation of Phosphotungstic Heteropoly Acid Quaternary Ammonium Salt Catalyst:

[0026] Take hexadecyltrimethylammonium bromide as an example to prepare phosphotungstic heteropolyacid quaternary ammonium salt catalyst:

[0027] Add 20 grams of tungstic acid (80 mmol) and 85 ml of 30% mass percent concentration of hydrogen peroxide (832.5 mmol) into the reactor, stir and heat to 60 ° C, react for 80 minutes, cool to room temperature, and then add 2.32 grams of mass Percentage concentration is that the phosphoric acid (20mmol) of 85% is dissolved in 9ml water and adds in the reaction solution, continues to stir after 50 minutes with 210ml distilled water dilution this reaction solution; In 500ml of chloroform, add dropwise to the above reaction solution, and continue to stir for 80 minutes, static layering, separate the organic phase and distill under reduced pressure to remove the solvent in the organic phase, and the residue is heated at 60°C Vacuum drying promptly ...

Embodiment 1

[0031] In a 250ml four-necked flask, add 125ml 1,2-dichloroethane, 25ml (0.185mol) dicyclopentadiene, 0.99 grams (5.1×10 -4 mol) Catalyst 2, the hydrogen peroxide of 27.2ml weight percent concentration 50% (0.472mol) is added dropwise in the reaction bottle, and make the temperature in the reactor can not exceed 50 ℃, after hydrogen peroxide dropwise, at 60 ℃ Continue to react under the conditions for 12 hours, take 2ml samples directly from the reactor with a pipette for analysis, recover 1,2-dichloroethane by distillation under reduced pressure, cool to room temperature to remove the water in the reactor, and then use 250ml ethyl acetate The ester was divided into two times to dissolve the residue and filtered to obtain the catalyst. The filtrate was distilled under reduced pressure to recover the ethyl acetate organic solvent to obtain a crude product, which was then recrystallized using a mixed solvent of ethyl acetate and petroleum ether with a volume ratio of 1:4 to obtai...

Embodiment 2

[0033] In a 250ml four-necked flask, add 54ml toluene, 18.0ml (0.1335mol) dicyclopentadiene, 1.0 grams (5.1×10 -4 mol) Catalyst 3, 33ml of hydrogen peroxide with a weight percent concentration of 30% (0.3232mol), after the hydrogen peroxide has been added dropwise, continue the reaction at 80°C for 6 hours, and take 2ml of the sample directly from the reactor with a pipette To be analyzed, filter the reacted material, reclaim the toluene from the filtrate by distillation under reduced pressure, remove the remaining water after cooling to room temperature, then use 100ml ethyl acetate to dissolve the residue twice and filter to obtain the catalyst, and distill the filtrate under reduced pressure The crude product was obtained after recovering the ethyl acetate organic solvent, and then recrystallized using a mixed solvent of ethyl acetate and petroleum ether with a volume ratio of 1:5 to obtain a white powdery solid, and the others were the same as in Example 1 and omitted.

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Abstract

The invention discloses a catalytic preparation method of dicyclopentadiene dioxide by quaternary ammonium heteropoly phosphato tungstate, which is characterized by comprising the following steps: epoxidation reaction: adding the raw materials of dicyclopentadiene, solvent I and quaternary ammonium heteropoly phosphato tungstate in a reactor, heating the temperature to 30-80 DEG C, stirring and dropwise adding aqueous hydrogen peroxide solution, and reacting for 3-36h under the temperature of 30-80 DEG C after dropwise adding; post-treatment: cooling the reacted materials to room temperature, evaporating solvent I by reduced pressure distillation and separating and removing water to obtain the mixture of the product and the quaternary ammonium heteropoly phosphato tungstate catalyst, dissolving and filtering the mixture by ethyl acetate to obtain filter cake, namely the recovered quaternary ammonium heteropoly phosphato tungstate catalyst, recovering ethyl acetate by performing reduced pressure distillation on filtrate to obtain the crude product, performing recrystallization on the crude product by solvent II, and drying to obtain the product. The invention has the advantages of convenient operation, high safety, small pollution, simple post treatment, and high product yield and purity.

Description

technical field [0001] The invention belongs to organic epoxy compounds, and relates to a method for preparing dicyclopentadiene dioxide by catalyzing a quaternary ammonium salt of phosphotungstic heteropolyacid. Background technique [0002] Dicyclopentadiene dioxide (or Dicyclopentadiene Dioxide, domestic trade name R-122, EP 207; English name: Dicyclopentadiene dioxide; Bicyclopentadienedioxide) is an alicyclic epoxide with excellent performance. It has excellent weather resistance, heat resistance, high hardness, and good electrical insulation performance. It is used in high temperature resistant casting materials, glass fiber reinforced plastics, adhesives, laminated materials, and electronic device packaging. Dicyclopentadiene dioxide is generally prepared by epoxidation of dicyclopentadiene, and the raw materials are easily available. In the prior art, the traditional methods for preparing olefin epoxides include the chlorohydrin method and the peracid method. These ...

Claims

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Application Information

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IPC IPC(8): C07D493/08
Inventor 吴学明李学超唐安斌李建学杨波
Owner SICHUAN DONGFANG INSULATING MATERIAL
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