Preparation method of meta-aminophenol-formaldehyde resin spheres and preparation method of carbon spheres

A technology of m-aminophenol and formaldehyde resin, applied in the polymer field, can solve the problems of low product yield, rough surface, complicated synthesis steps and post-processing, etc., and achieve the effect of high yield and high monodispersity.

Active Publication Date: 2012-08-22
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Abstract
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Problems solved by technology

Recently, a method for preparing phenolic resin spheres and corresponding carbon spheres by a synthetic method of oxazidine was reported in the literature (J.Am.Chem.Soc.2011, 133, 15304-15307.), by adjusting the synthesis temperature to obtain Resin spheres and corresponding carbon spheres, but the particle size range of resin spheres and carbon spheres obtained by this method is small, the adjustability of particle size is small, the yield of the obtained product is small, and, in the process of preparation The use of surfactants in the method makes the synthesis steps and post-processing more cumbersome
[0004] In order to simplify the preparation process of phenolic resin spheres and carbon spheres and improve the performance of phenolic resin spheres and carbon spheres, the prior art discloses a Method for synthesizing resorcinol-formaldehyde resin spheres and corresponding carbon spheres (Angew.Chem., Int.Ed.2011, 50, 5947-5951.), however, the resorcinol-formaldehyde resin obtained by this method The surface of the spheres and corresponding carbon spheres is rough and the monodispersity is low, which is not conducive to the application of resin spheres and carbon spheres

Method used

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  • Preparation method of meta-aminophenol-formaldehyde resin spheres and preparation method of carbon spheres
  • Preparation method of meta-aminophenol-formaldehyde resin spheres and preparation method of carbon spheres
  • Preparation method of meta-aminophenol-formaldehyde resin spheres and preparation method of carbon spheres

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preparation example Construction

[0029] The invention provides a kind of preparation method of m-aminophenol-formaldehyde resin ball, comprises the following steps:

[0030] Catalyst, m-aminophenol and formaldehyde are dissolved in solvent, and m-aminophenol-formaldehyde resin balls are obtained after polymerization;

[0031] The catalyst is ammonia and / or ethylenediamine;

[0032] The solvent is an aqueous solution, an alcoholic solution or a mixed solution of water and alcoholic compounds.

[0033] In the present invention, firstly, the catalyst, m-aminophenol and formaldehyde are dissolved in a solvent to obtain a mixed solution, and the catalyst is ammonia water and / or ethylenediamine, preferably ammonia water. In the present invention, there is no special limitation on the order in which the catalyst, m-aminophenol and formaldehyde are dissolved in the solvent, and the technical solution for preparing phenolic resin well known to those skilled in the art can be used. In the present invention, the m-ami...

Embodiment 1

[0053] Add 32.7 mg of m-aminophenol to a mixed solution of 12 mL of water and 4.8 mL of methanol, stir and dissolve at 30 °C for 10 minutes, then add 0.6 μL of ammonia water with a mass concentration of 28%, and then stir the resulting mixed solution for 20 Minutes later, 46 μL of formaldehyde was added thereto, and after stirring for 4 hours, the resulting mixed solution was placed in a 20 mL reaction kettle, and stirred at 100° C. for 24 hours. The obtained reaction product was centrifuged at 8000 rpm for 5 minutes, the centrifuged solid was washed twice with water, and dried at 80° C. for 12 hours to obtain m-aminophenol-formaldehyde resin balls.

[0054] The mass of the m-aminophenol-formaldehyde resin balls weighed by the present invention is 47.7 mg, and the calculated yield is 94%. The present invention carries out scanning electron microscope scanning analysis to the m-aminophenol-formaldehyde resin ball obtained, the result is as follows figure 1 as shown, figure 1 ...

Embodiment 2

[0060] Add 32.7 mg of m-aminophenol to a mixed solution of 12 mL of water and 4.8 mL of methanol, stir and dissolve at 30°C for 10 minutes, then add 12 μL of ammonia water with a mass concentration of 28%, and then stir the resulting mixed solution for 20 minutes 46 μL of formaldehyde was added thereto, and after stirring for 4 hours, the resulting mixed solution was placed in a 20 mL reaction kettle, and stirred at 100° C. for 24 hours. The obtained reaction product was centrifuged at 8000 rpm for 5 minutes, the centrifuged solid was washed twice with water, and dried at 80° C. for 12 hours to obtain m-aminophenol-formaldehyde resin balls.

[0061] The mass of the m-aminophenol-formaldehyde resin balls weighed in the present invention is 46.6 mg, and the calculated yield is 92.0%. The present invention carries out scanning electron microscope scanning analysis to the m-aminophenol-formaldehyde resin ball obtained, the result shows that the phenolic resin ball prepared by the ...

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Abstract

The invention provides a preparation method of meta-aminophenol-formaldehyde resin spheres and a preparation method of carbon spheres. Meta-aminophenol and formaldehyde are subjected to polymerization reaction in the presence of ammonia water and/or ethylene diamine. In the polymerization reaction process, the formaldehyde, the meta-aminophenol and the ammonia water and/or ethylene diamine as the catalyst form a micelle in the solvent; in the micelle, the meta-aminophenol and the formaldehyde are subjected to polymerization reaction under the catalytic action of the ammonia water and/or ethylene diamine to obtain the meta-aminophenolformaldehyde resin spheres; and meanwhile, part of the ammonia water and/or ethylene diamine are/is distributed on the surface of the micelle to form positive charges, and the electrostatic repulsion action inhibits the bonding of the micelle. Thus, the obtained meta-aminophenol-formaldehyde resin spheres have high monodispersity, and the dimensions of the resin spheres can be adjusted within a wide range. The meta-aminophenol-formaldehyde resin spheres are calcined to obtain the corresponding carbon spheres, and the carbon spheres also have high monodispersity, thereby being beneficial to the application of the carbon spheres.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a method for preparing m-aminophenol-formaldehyde resin spheres and a method for preparing carbon spheres. Background technique [0002] Monodisperse colloidal spheres are widely used in the synthesis of particle size reference materials, photonic crystals, ordered macroporous materials, macroporous catalysts, and proton membrane composites due to their single shape and controllable size. For example, drug delivery, medical diagnostics, alternate catalysts, complex structures and nanodevices. For the preparation of monodisperse colloidal spheres, the prior art discloses a pyrolysis method and a template method, but these two methods require high equipment and are inconvenient for post-processing, so they are not suitable for large-scale synthesis of carbon spheres. In order to simplify the synthesis steps of monodisperse colloidal spheres, some polymer spheres, such as polystyr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/08C08G8/16C01B31/02C01B32/05
Inventor 徐国宝赵建明
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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