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Autocatalysis preparation method of copolymer benzoxazine-resin polymer sphere and autocatalysis preparation method of resin-based carbon sphere

A technology of benzoxazine and polymer balls, applied in the field of polymers, can solve the problems of low monodispersity, complicated synthesis steps and post-processing, and small particle size range of resin balls and carbon balls.

Active Publication Date: 2016-01-27
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, during the polymerization process, ammonia water may not only act as a catalyst, the resulting resorcinol-formaldehyde resin spheres and corresponding carbon spheres have rough surfaces and low monodispersity, which is not conducive to the application of resin spheres and carbon spheres.
Based on benzoxazine chemistry, a novel highly uniform polybenzoxazine-based resin polymer nanospheres prepared by Mannich condensation of resorcinol, formaldehyde and 1,6-hexanediamine was reported (J. Am.Chem.Soc.2011,133,15304-15307.), during the preparation process, they used block copolymer F127 to adjust the shape of the ball, and obtained the resin ball and the corresponding carbon ball by adjusting the synthesis temperature, but this method The particle size range of the obtained resin balls and carbon balls is small, the adjustability of the particle size is small, and the product concentration per unit volume of the obtained product is small, and a surfactant is used in the preparation process, so that the synthesis steps and post-processing steps are relatively small. More cumbersome to deal with

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  • Autocatalysis preparation method of copolymer benzoxazine-resin polymer sphere and autocatalysis preparation method of resin-based carbon sphere
  • Autocatalysis preparation method of copolymer benzoxazine-resin polymer sphere and autocatalysis preparation method of resin-based carbon sphere
  • Autocatalysis preparation method of copolymer benzoxazine-resin polymer sphere and autocatalysis preparation method of resin-based carbon sphere

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preparation example Construction

[0039] The invention provides a self-catalyzed preparation method of copolymerized benzoxazine-resin polymer spheres, comprising the following steps:

[0040] dissolving m-aminophenol and formaldehyde in a solvent, and obtaining copolymerized benzoxazine-resin polymer balls after polymerization;

[0041] The solvent is a mixed solution of water and alcohol compounds.

[0042] In the present invention, m-aminophenol and formaldehyde are firstly dissolved in a solvent to obtain a mixed solution, and no external catalyst is added in the process. In the present invention, there is no special limitation on the order in which 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-aminophenol is preferably firstly added to the solvent, and then formaldehyde is added thereto to obtain a mixed solution. After the formaldehyde is added, m-am...

Embodiment 1

[0062] Add 73.33 mg of m-aminophenol to a mixed solution of 8.4 mL of water and 8.4 mL of methanol, stir and dissolve at 30°C for 10 minutes, then add 121 μL of formaldehyde, stir for 1 hour, then raise the temperature of the water bath to 75°C , and continued to stir for 4 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 copolymerized benzoxazine-resin polymer balls.

[0063] The present invention carries out scanning electron microscope scanning analysis to the obtained copolymerized benzoxazine-resin polymer ball, and the result is as follows figure 1 as shown, figure 1 The scanning electron micrograph of the copolymerized benzoxazine-resin polymer sphere prepared for Example 1 of the present invention is obtained by figure 1 It can be seen that the phenolic resin balls prepared by the present invention have high monodispersity. The present inventi...

Embodiment 2

[0065] Add 73.33 mg of m-aminophenol to a mixed solution of 8.4 mL of water and 8.4 mL of methanol, stir and dissolve at 20°C for 10 minutes, then add 121 μL of formaldehyde, stir for 1 hour, then raise the temperature of the water bath to 75°C , and continued to stir for 4 hours. The obtained reaction product was centrifuged at 8000 rpm for 5 minutes, washed twice with centrifuged water, and then dried at 80° C. for 12 hours to obtain copolymerized benzoxazine-resin polymer balls.

[0066] The present invention carries out scanning electron microscope scanning analysis to the obtained copolymerized benzoxazine-resin polymer ball, and the result is as follows Figure 8 as shown, Figure 8 The scanning electron micrograph of the copolymerized benzoxazine-resin polymer sphere prepared for Example 2 of the present invention is obtained by Figure 8 It can be seen that the phenolic resin balls prepared by the present invention have high monodispersity. The particle diameter of ...

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Abstract

The invention provides an autocatalysis preparation method of a copolymer benzoxazine-resin polymer sphere and belongs to the technical field of polymers. According to the method, on the condition that no catalyst is added, m-aminophenol and formaldehyde are dissolved in a solvent, and after a polymerization reaction, the copolymer benzoxazine-resin polymer sphere is obtained; the solvent is a mixed solution of water and alcohol compounds. The invention further provides a preparation method of a copolymer benzoxazine-resin-based carbon sphere; the method comprises the step that the obtained copolymer benzoxazine-resin polymer sphere is sintered to obtain the corresponding carbon sphere. The obtained copolymer benzoxazine-resin polymer sphere and carbon sphere have the high monodispersity, the size of the resin sphere can be adjusted in a wide range, and the application of the resin sphere is facilitated. The copolymer benzoxazine-resin polymer sphere prepared through the method has the high concentration in a unit reaction system.

Description

technical field [0001] The invention belongs to the technical field of polymers, and in particular relates to a self-catalyzed preparation method of copolymerized benzoxazine-resin polymer balls and a self-catalyzed preparation method of resin-based carbon balls. Background technique [0002] In recent years, molecular level design and controllable preparation of monodisperse colloidal spheres have become research hotspots, including silica spheres, polymer spheres, carbon spheres and their composite spheres, mainly because they have a wide range of applications, such as: colloidal Catalysis, photonic crystals, drug delivery, biosensing, energy storage and templating agents, etc. The application of these colloidal spheres is closely related to their size, structure and composition. Carbon spheres are different from most polymer spheres and silica spheres, they have large specific surface area, high thermodynamic stability (in an inert environment) and strong acid and alkali...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C01B31/02
Inventor 徐国宝赵建明
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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