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Solid supported heteropoly acid catalyst and preparation method thereof

A technology for immobilizing heteropolyacids and catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of poor synthesis process safety, low yield, catalyst residues, etc. Long life, high catalytic activity and easy recycling

Active Publication Date: 2011-11-02
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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  • Solid supported heteropoly acid catalyst and preparation method thereof
  • Solid supported heteropoly acid catalyst and preparation method thereof
  • Solid supported heteropoly acid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Embodiment 1 The preparation technology of this immobilized phosphotungstic acid catalyst is as follows:

[0027] Add 2 Kg of chloromethyl polystyrene resin to 61 N, N-dimethylformamide (DMF) to swell for 2 hours, then add 8 L of 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 expressed as respectively in Represents chloromethyl polystyrene resin carrier.

[0028] 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 reaction temperature at about 60°C, react for 2.5 hours, adjust the pH value of the...

Embodiment 2

[0039] The preparation technology of embodiment 2 this immobilized phosphomolybdic acid catalyst is as follows:

[0040] Add 1.5Kg of bromomethyl polystyrene resin to 5L of N,N-dimethylformamide (DMF) to swell for 3h, then add 6L of pyridine or its homologous compound and stir for 20h at a temperature of 80-90°C, and then react The mixture is cooled, filtered with suction, and the filter cake is washed with water and ethanol in sequence, 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;

[0041] 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 the reaction solution to <2 with dilute hydrochloric acid, and then cool the mixed reaction solution to r...

Embodiment 3

[0043] Embodiment 3 The preparation technology of this immobilized phosphovanadic acid catalyst is as follows:

[0044] Add 200g of fluoromethyl polystyrene resin to 0.5L of dimethyl sulfoxide (DMSO) to swell for 4h, then add 0.3L of piperidine or its homologous compound and stir for 18h at a temperature of 100°C, then cool the reaction mixture and pump Filter, the filter cake is successively washed with water, and after ethanol washing, then extract with ethanol for 10h, and then vacuum-dry 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 <2 with dilute hydrochloric acid, and then cool the mixed reaction solution to room temperature. T...

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Abstract

The invention relates to an immobilization heteropoly acid catalyst and a method for preparing the same. The method comprises that: halogenating methyl polystyrene resins and compounds containing active tertiary amine radicals are dispersed in an organic solvent and react under the condition of heating, and the reaction product treated forms an immobilization quaternary ammonium salt resin; phosphotungstic acid, phosphomolybdic acid or vanadic acid is treated in an acid water solution with an oxidant, and added with the immobilization quaternary ammonium salt resin for reaction, the reaction product is washed and dried to prepare the immobilization heteropoly acid catalyst; and the weight ratio of the active heteropolyacid catalyst radicals contained in the immobilization heteropoly acid catalyst to the carrier of the active heteropoly acid catalyst radicals is 1:2-5. The catalyst and the method have the advantages of high catalytic activity, easy recovery, simple preparation method and long service life, and can effectively improve product yield and purity of the alicyclic ring epoxy resin synthesis process, simplify the synthesis process, make the synthesis process more environment friendly and safe, reduce production cost and is applied to large-scale industrialized production.

Description

technical field [0001] The invention relates to a catalyst used in the synthesis process of epoxy resin, in particular to a solid-loaded heteropolyacid catalyst and a preparation method thereof. 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 more commonly used preparation process of cycloaliphatic epoxy resin is the catalytic oxidation method, which mainly uses a homogeneous heteropolyacid catalyst as a catalyst, and uses hyd...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/188B01J27/19B01J27/198C08G59/68
Inventor 穆学军吴国文李钧邱子皓周文杰
Owner NANTONG SYNASIA NEW MATERIAL CO LTD