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Process for producing sea urchin shaped polyaniline microsphere supported catalyst

A supported catalyst, polyaniline technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., can solve the problem of reduced cleaning times, monomer diffusion, and poor control , increase processing steps and other issues, to achieve the effect of simple preparation method, easy separation and high catalytic efficiency

Inactive Publication Date: 2009-04-08
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the problem with this method is that after the aniline monomer is loaded by the osmosis method, a centrifugal cleaning step is required to remove the monomer solution on the outside and the surface of the ball, and then the microspheres loaded with the monomer in the cavity are dispersed into the aqueous oxidant solution, and the centrifugal cleaning increases Too many cleaning times and too long time will reduce the diffusion of monomers in the microspheres, and too few cleaning times will lead to excessive monomer retention in the outer gap and outer surface of the balls, which will affect the product morphology

Method used

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  • Process for producing sea urchin shaped polyaniline microsphere supported catalyst
  • Process for producing sea urchin shaped polyaniline microsphere supported catalyst
  • Process for producing sea urchin shaped polyaniline microsphere supported catalyst

Examples

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Embodiment 1

[0020] 1. Preparation of sea urchin-like polyaniline composite microspheres

[0021] 1) Monodisperse polystyrene microspheres are prepared by a soap-free emulsion polymerization method;

[0022] 2) Disperse the polystyrene microspheres synthesized in step 1) into deionized water to form 10gL -1 Emulsion, measure aniline monomer and add to the above emulsion, the concentration of aniline monomer is 15gL -1 , swell for 5 hours under magnetic stirring at 10°C;

[0023] 3) According to the molar ratio of the oxidizing agent to the monomer being 1:2, the oxidizing agent ferric nitrate was added to the mixed solution in step 2), reacted at 40°C for 12 hours, then centrifuged, washed with distilled water and absolute ethanol in turn, and dried The dark green sea urchin-like polyaniline composite microspheres were obtained.

[0024] The prepared sea urchin-like polyaniline composite microspheres as figure 1 As shown, the diameter of the fiber is 15-30nm, the average length is 60-9...

Embodiment 2

[0029] 1. Preparation of sea urchin-like polyaniline composite microspheres

[0030] 1) Monodisperse polystyrene microspheres are prepared by a soap-free emulsion polymerization method;

[0031] 2) Disperse the polystyrene microspheres synthesized in step 1) into deionized water to form 15gL -1 Emulsion, measure aniline monomer and add to the above emulsion, the concentration of aniline monomer is 75gL -1 , swell for 5 hours under magnetic stirring at 20°C;

[0032] 3) According to the molar ratio of the oxidizing agent to the monomer being 1:4, add the oxidizing agent ferric chloride to the mixed solution in step 2), react at 20°C for 20 hours, then centrifuge, wash with distilled water and absolute ethanol in turn, and dry Finally, dark green sea urchin-like polyaniline composite microspheres were obtained.

[0033] The prepared sea urchin-like polyaniline composite microspheres as figure 2 As shown, the diameter of the fiber is 20-50nm, the average length is 40-80nm, a...

Embodiment 3

[0038] 1. Preparation of sea urchin-like polyaniline composite microspheres

[0039] 1) Monodisperse polystyrene microspheres are prepared by a soap-free emulsion polymerization method;

[0040] 2) Disperse the polystyrene microspheres synthesized in step 1) into deionized water to form 20gL -1 Emulsion, measure aniline monomer and add to the above emulsion, the concentration of aniline monomer is 100gL -1 , swell for 6 hours under magnetic stirring at 30°C;

[0041] 3) According to the molar ratio of the oxidizing agent to the monomer being 1:4, the oxidizing agent ferric sulfate was added to the mixed solution in step 2), reacted at 30°C for 30 hours, then centrifuged, washed with distilled water and absolute ethanol in turn, and dried The dark green sea urchin-like polyaniline composite microspheres were obtained.

[0042] The prepared sea urchin-like polyaniline composite microspheres as image 3 As shown, the diameter of the fiber is 5-40nm, the average length is 70-1...

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Abstract

The invention provides a method for preparing a sea urchin like polyaniline microspheres supported catalyst, which belongs to the technical field of polymer supported catalytic material preparation, wherein polystyrene microspheres prepared by a soap-free emulsion polymerization method are used as seeds, and sea urchin like polyaniline microspheres are prepared by a seed swelling polymerization method. The method comprises the following steps: firstly, adding aniline monomers into aqueous solution of the polystyrene microspheres, stirring the mixture for a period of time so that the aniline monomers are swelled into the polystyrene microspheres; secondly, adding the mixture into aqueous solution of iron-based oxidants so that the aniline monomers swelled into the polystyrene microspheres can react with the oxidants so as to obtain the sea urchin like polyaniline composite microspheres; and thirdly, using a catalyst MoO2(acac)2 to perform load reaction with the prepared sea urchin like polyaniline composite microspheres to syntheize a polyaniline supported molybdenum-based catalyst. When the prepared polyaniline supported molybdenum-based catalyst is used for catalyzing cyclooctene to perform epoxidation, and tert-butyl hydroperoxide is used as an oxygen source, and good catalytic activity and the recycling performance are represented.

Description

technical field [0001] The invention belongs to the technical field of preparation of polymer-loaded catalytic materials, and in particular relates to a preparation method of sea urchin-shaped polyaniline composite microspheres and a loaded catalyst thereof. Background technique [0002] Epoxy compounds (such as propylene oxide, epichlorohydrin, styrene oxide) are important intermediates in organic synthesis, and are widely used in petrochemical, fine chemical, organic synthesis, pharmaceutical, spice and electronic industries. The most important way to prepare epoxides is olefin epoxidation, so epoxidation plays an important role in both organic synthesis and chemical industry, and has always been a research hotspot. Traditional organic oxidation reactions have disadvantages such as expensive raw materials, long reaction time, serious waste of resources, etc., which limit their wide application in industry. Therefore, the environmentally friendly, economical and reasonable...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J31/04C07D301/04
Inventor 王戈杨穆曹利静丁杭军孙冬柏
Owner UNIV OF SCI & TECH BEIJING
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