Method for synthesis of alicyclic epoxy resin with catalysis of solid supported heteropoly acid catalyst

A technology of immobilized heteropolyacid and epoxy resin, which is applied in the field of immobilized heteropolyacid catalyst to catalyze the synthesis of alicyclic epoxy resin, can solve the problems of low yield, poor synthesis process safety, catalyst residue, etc. The effect of high efficiency and purity, low cost and good safety

Active Publication Date: 2009-07-29
NANTONG SYNASIA NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of method that solid-loaded heteropolyacid catalyst catalyzes the synthesis of alicyclic epoxy resin, to overcome the alicyclic epoxy resin synthesis process security that exists in the prior art, low yield and catalyst residue And other issues

Method used

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  • Method for synthesis of alicyclic epoxy resin with catalysis of solid supported heteropoly acid catalyst
  • Method for synthesis of alicyclic epoxy resin with catalysis of solid supported heteropoly acid catalyst
  • Method for synthesis of alicyclic epoxy resin with catalysis of solid supported heteropoly acid catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1 The process for the synthesis of epoxy resin ERL-4221 catalyzed by the immobilized heteropolyacid catalyst is as follows:

[0025] Synthesis of immobilized phosphotungstic acid catalyst: add 2Kg chloromethyl polystyrene resin to 6L N,N-dimethylformamide (DMF) to swell for 2 hours, then add 8L tertiary amine R 1 R 2 R 3 N(R 1 , R 2 , R 3 is alkyl, cycloalkyl or benzyl) at 90-100°C for 24 hours, then cooled the reaction mixture, filtered it with suction, and washed the filter cake with water and ethanol in turn, then extracted with ethanol for 8-10 hours, and then vacuumed Dry to constant weight, make immobilized quaternary ammonium resin, this immobilized quaternary ammonium resin can be represented as respectively or in Represents chloromethyl polystyrene resin carrier;

[0026] Weigh 825g of phosphotungstic acid and dissolve it in 10L of water, stir the reaction, and take 1.5L of 30% H 2 o 2 Add to the reaction solution in 5 times, control the re...

Embodiment 2

[0037] Example 2 The process of the solid-supported heteropolyacid catalyst catalyzing the synthesis of dicyclopentadiene dioxide is as follows:

[0038]

[0039] Synthesis of immobilized phosphomolybdic acid catalyst: add 1.5Kg of bromomethyl polystyrene resin to 5L of dimethyl sulfoxide (DMSO) to swell for 3 hours, then add 6L of pyridine or its homologous compounds and stir at a temperature of 80-90°C After 20 hours, the reaction mixture was cooled, filtered with suction, and the filter cake was washed with water and ethanol in turn, then extracted with ethanol for 9 to 10 hours, and then dried in vacuum to constant weight to obtain a solid-loaded quaternary ammonium salt resin;

[0040] Take by weighing 30g phosphomolybdic acid and be dissolved in 500mL water, stir reaction, and take 350mL mass percent concentration and be 50% H 2 o 2 Add to the reaction solution in 5 times, control the reaction temperature at about 20°C, react for 6 hours, and adjust the pH value of t...

Embodiment 3

[0042] Embodiment 3 The technological process of this immobilized heteropolyacid catalyst catalytic synthesis of 4-vinyl epoxycyclohexane is as follows:

[0043]

[0044] Synthesis of immobilized phosphovanadic acid catalyst: add 200g fluoromethyl polystyrene resin to 0.5L N,N-dimethylformamide (DMF) to swell for 4h, then add 0.3L piperidine or its homologous compound at 100°C Stir at high temperature for 18 hours, then cool the reaction mixture, filter with suction, wash the filter cake with water and ethanol in turn, then extract with ethanol for 10 hours, and then dry it in vacuum to constant weight to obtain a solid-loaded quaternary ammonium salt resin;

[0045] Take by weighing 10g phosphovanadic acid and be dissolved in 150mL water, stir reaction, and take 120mL mass percent concentration and be 40% H 2 o 2 Add to the reaction solution in 5 times, control the reaction temperature at about 50°C, react for 3 hours, and adjust the pH value of the reaction solution to <...

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Abstract

The invention relates to a method for using a solid borne heteropoly acid catalyst to catalyze and synthesize alicyclic epoxy resin. The method comprises the following steps: halogenated methane polystyrene resin and compound with active tertiary amine groups are dissolved in an organic solvent and react to form solid borne quaternary ammonium salt resin; H3PO4OM12 xH2O is treated in acidic aqueous solution by an oxidizer and reacts with the solid borne quaternary ammonium salt resin, wherein, M is tungsten, molybdenum or vanadium, and then the solid borne heteropoly acid catalyst is prepared; the solid borne heteropoly acid catalyst, unsaturated alicyclic compound and a cocatalyst are dissolved in the organic solvent, then the oxidizer is added to form acidic mixed reacting solution, stirring is carried out continuously till the reaction is completed, the solid borne heteropoly acid catalyst is recovered and the filtrate is cleaned to remove the organic solvent and then the alicyclic epoxy resin is obtained. The invention has high yield and purity, safe and simple technique, convenient operation and low cost, is environment-friendly and is completely suitable for industrial production on large scale.

Description

technical field [0001] The invention relates to a preparation process of an alicyclic epoxy resin, in particular to a method for catalytically synthesizing an alicyclic epoxy resin with a solid-loaded heteropolyacid catalyst. Background technique [0002] Epoxy resin is an important thermosetting resin variety, which is widely used in chemical industry, light industry, water conservancy, transportation, machinery, electronics, home appliances, automobiles, aerospace and other industrial fields. As a new generation of epoxy resin, cycloaliphatic epoxy resin is suitable for outdoor use due to its structural characteristics, good electrical insulation, weather resistance, UV resistance and electronic radiation resistance, and can be widely used Anti-ultraviolet coatings and electronic products such as LEDs. At present, the commonly used preparation technology of cycloaliphatic epoxy resin is mainly peroxyacid oxidation method and catalytic oxidation method. Epoxidation reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/68
Inventor 穆学军吴国文李钧邱子皓周文杰
Owner NANTONG SYNASIA NEW MATERIAL CO LTD
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