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Preparation method for benzoxazine resin nano-polymer sphere and benzoxazine resin nano-polymer carbon sphere

A nanopolymer and benzoxazine technology, applied in the field of controllable preparation of spherical nanomaterials, can solve the problems of uneven product size, difficult separation and purification, complicated operation, etc., and achieve uniform particle size, simple and fast operation, and high purity high effect

Inactive Publication Date: 2013-07-31
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] At present, there are chemical vapor deposition, plasma deposition, catalytic pyrolysis, direct thermal condensation method, liquid phase emulsification method, suspension method and other methods for the synthesis of nano carbon spheres, but most of the synthesis methods have high energy consumption, expensive equipment, or complicated operation. The size of the product is uneven, or it is only a by-product of some reactions, so it is difficult to separate and purify

Method used

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  • Preparation method for benzoxazine resin nano-polymer sphere and benzoxazine resin nano-polymer carbon sphere
  • Preparation method for benzoxazine resin nano-polymer sphere and benzoxazine resin nano-polymer carbon sphere
  • Preparation method for benzoxazine resin nano-polymer sphere and benzoxazine resin nano-polymer carbon sphere

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Experimental program
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Effect test

Embodiment 1

[0025] Weigh 0.11g resorcinol and put it into a round bottom flask, add 50ml deionized water and stir at room temperature, add 0.05g surfactant F127 (produced by Fluka company) after dissolving, add 146μl 37% formaldehyde solution and 0.029 1,6-g of 1,6-hexamethylenediamine, continue to stir, after the white colloid is obtained, the above reaction solution is moved to a water bath at 80°C, and stirred for 24 hours to obtain an aqueous solution of monodisperse nano-polymer spheres, after 12000r / min After centrifugation for 10 min, wash with water and ethanol, and dry the product at room temperature or in an oven at 50°C overnight.

[0026] The obtained nanometer polymer sphere diameter of the present embodiment is 180 ± 10nm, and its scanning electron microscope is as follows: figure 1 shown.

Embodiment 2

[0028] Place the nanometer polymer balls prepared in Example 1 into a carbonization furnace for carbonization, and use an inert gas protection to rise from room temperature to 400°C at a rate of 1-3°C / min, and dry at a constant temperature for 60 minutes; The rate was increased from 400°C to the final carbonization temperature of 900°C, and the temperature was kept constant for 60 minutes to obtain carbonized nano-carbon spheres with shape retention.

[0029] The particle size of nano carbon spheres obtained in this embodiment is 160 ± 5nm, and its scanning electron microscope is as follows: figure 2 As shown, its BET specific surface area is 635m 2 g -1 , micropore volume 0.27cm 3 g -1 .

Embodiment 3

[0031] Weigh 0.11g of resorcinol into a round bottom flask, add 50ml of deionized water and stir at room temperature, add 0.01g of surfactant F127 after dissolving, add 146μl of 37% formaldehyde solution and 33μl of ethylenediamine after stirring completely, Continue stirring to obtain a white colloid, move the above reaction solution to a water bath at 80°C, and stir for 24 hours to obtain an aqueous solution of monodisperse nano-polymer spheres, centrifuge at 12000r / min for 10min, wash with water and ethanol, and The product was dried overnight at room temperature or in an oven at 50 °C.

[0032] The diameter of the nano-polymer spheres prepared in this example is 700±50 nm.

[0033] The above-mentioned nano-polymer spheres are placed in a carbonization furnace for carbonization to obtain nano-polymer carbon spheres with a particle size of 550±20nm and a BET specific surface area of ​​610m 2 g -1 , micropore volume 0.26cm 3 g -1 .

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Abstract

The invention discloses a preparation method for benzoxazine resin nano-polymer sphere and benzoxazine resin nano-polymer carbon sphere. The preparation method is characterized by: adopting a phenol, an aldehyde and a amine as raw materials, adopting water as a solvent, carrying out a low-temperature polymerization to prepare the monodisperse benzoxazine resin nano-polymer sphere; placing the benzoxazine resin nano-polymer sphere in a carbonization furnace, followed by carrying out a carbonization in the protection of inert gas to prepare the monodisperse nano-polymer carbon sphere. With the preparation method provided by the present invention, operation is simple, required equipment is simple, and the monodisperse benzoxazine resin nano-polymer sphere with uniform size and the monodisperse benzoxazine resin nano-polymer carbon sphere with uniform size are prepared.

Description

technical field [0001] The present invention relates to the field of controllable preparation of spherical nanomaterials, and more specifically relates to a simple method for preparing monodisperse, size-controllable, nitrogen-enriched nano-polymer spheres, and carbonizing the nano-polymer spheres as precursors to obtain nano Carbon ball technology. Background technique [0002] Spherical nanomaterials have attracted extensive attention and applications because of their unique morphology and excellent performance. Spherical structure, particle size from tens of nanometers to tens of microns, monodisperse spherical materials have been widely used in adsorption, catalyst carrier, photonic crystal, drug sustained release, nano-devices, gas storage and energy storage, lubricants, etc. . Common monodisperse spherical nanomaterials include inorganic oxide spheres, organic polymer spheres, carbon spheres, etc. [0003] At present, inorganic oxide spheres such as silicon oxide sp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06C01B31/02B82Y40/00B01J31/28C07C47/54C07C45/38B01J20/20B01J20/26A61K47/04A61K47/34
Inventor 陆安慧李文翠王帅郝广平钱旦
Owner DALIAN UNIV OF TECH
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