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Preparation method for boron-containing phenolic resin microsphere and carbon microsphere

A technology of boron phenolic resin and microspheres, which is applied in the field of preparation of boron-containing phenolic resin microspheres and carbon microspheres, can solve the problems of deformation of carbonized products, low carbonization yield of microspheres, and insufficient heat resistance of microspheres, and achieve Effects of increasing carbonization yield and increasing reactivity

Active Publication Date: 2019-08-20
沙县宏盛塑料有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] However, in the prior art, the preparation of monodisperse nano-microspheres mainly uses highly reactive monomers, such as resorcinol, triaminophenol, melamine, etc., and other monomers are difficult to prepare monodisperse microspheres. The prepared microspheres generally have defects such as insufficient heat resistance, low carbonization yield of microspheres, and deformation of carbonized products.

Method used

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  • Preparation method for boron-containing phenolic resin microsphere and carbon microsphere
  • Preparation method for boron-containing phenolic resin microsphere and carbon microsphere
  • Preparation method for boron-containing phenolic resin microsphere and carbon microsphere

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preparation example Construction

[0025] The invention provides a method for preparing boron-containing phenolic resin microspheres. Firstly, an organoboron compound and an aldehyde are subjected to a prepolymerization reaction under acidic conditions, and then a polycondensation reaction is performed with an aldehyde and a curing agent under conditions of an alkaline catalyst and a solvent. , and finally placed in a high-pressure reactor to continue polycondensation and cross-linking to obtain boron-containing phenolic resin microspheres.

[0026] From the above description, it can be seen that the beneficial effect of the present invention is that the boron-containing phenolic resin microspheres are prepared by using the organoboron compound as the phenol source through a four-step method, which effectively increases the reactivity of the organoboron compound, the dispersibility and particle size of the microspheres It is well controlled and the carbonization yield of microspheres is significantly improved. ...

Embodiment 1

[0045] 1) Add 10g of triphenyl borate, 4g of 37% aqueous formaldehyde solution and 0.05g of oxalic acid into the reaction kettle, heat up to 90°C and react for 30min;

[0046] 2) Add 15 g of ammonia water, 400 mL of water and 15 g of 37% formaldehyde solution to the reactant obtained in step 1), and stir for 3 h;

[0047] 3) Add 5 g of hexamethylenetetramine to the reactant obtained in step 2), and stir for 12 h;

[0048] 4) Put the above solution into an autoclave and react at a temperature of 100°C for 48 hours;

[0049] 5) The product is washed with water and dried in vacuum to obtain boron-containing phenolic resin microspheres.

[0050] Carbonization: Place the phenolic resin microspheres in a carbonization furnace, raise the temperature to 800°C at a rate of 5°C / min under a nitrogen atmosphere, and keep it for 3 hours. After cooling down, phenolic resin-based carbon microspheres are obtained, with a yield of 79% %.

[0051] see figure 1 , is the SEM image of the prep...

Embodiment 2

[0053] 1) Add 10g of triphenyl borate, 10g of 37% formaldehyde solution and 0.06g of oxalic acid into the reaction kettle, heat up to 100°C and react for 10min;

[0054] 2) Add 15 g of ammonia water, 400 mL of water and 15 g of 37% formaldehyde solution to the reactant obtained in step 1), and stir for 3 h;

[0055] 3) Add 5 g of hexamethylenetetramine to the reactant obtained in step 2), and stir for 12 h;

[0056] 4) Put the above solution into an autoclave and react at a temperature of 100°C for 48 hours;

[0057] 5) The product is washed with water and dried in vacuum to obtain boron-containing phenolic resin microspheres.

[0058] Carbonization: Place the phenolic resin microspheres in a carbonization furnace, raise the temperature to 800°C at a rate of 5°C / min under a nitrogen atmosphere, and keep it for 3 hours. After cooling down, carbon microspheres are obtained with a yield of 78%.

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Abstract

The invention specifically relates to a preparation method for a boron-containing phenolic resin microsphere and a carbon microsphere, belonging to the field of chemical synthetic resin microspheres.The preparation method for the boron-containing phenolic resin microsphere comprises the following steps: firstly, subjecting an organoboron compound and aldehyde to prepolymerization under acidic conditions; then subjecting a product of the previous step to a polycondensation reaction with aldehyde and a curing agent under the conditions of a basic catalyst and a solvent; and finally putting a product of the previous step in an autoclave for further polycondensation and crosslinking to obtain the boron-containing phenolic resin microsphere. The invention has the beneficial effects that the preparation method for the boron-containing phenolic resin microsphere and the carbon microspheres in the invention employs the organic boron compound as a phenol source and prepares the boron-containing phenolic resin microsphere through four steps, so the reactivity of the organic boron compound is effectively increased, the dispersibility and particle size of the microsphere are well controlled,and the carbonization yield of the microspheres is significantly improved. According to testing results, the particle size of the microsphere prepared in the invention can be controlled to a range of1-1000 nm, and the yield of the carbonization product of the microsphere is 75% or more.

Description

technical field [0001] The invention relates to the field of chemical synthetic resin microspheres, in particular to a method for preparing boron-containing phenolic resin microspheres and carbon microspheres. Background technique [0002] Phenolic resin (PF) has rich sources of raw materials, low price, simple production process, excellent mechanical properties, heat resistance, electrical insulation, dimensional stability, molding processability and flame retardancy, good dimensional stability of products, electrical insulation With excellent performance and low smoke emission, it has become an indispensable material in the industrial sector, and has been widely used in related industries such as automobiles, home appliances, electrical appliances, steel and housing. However, with the development of industry, especially the development of aerospace and other cutting-edge defense technologies, new requirements have been put forward for phenolic resins, and scientific resear...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G79/08C01B32/05
CPCC08G79/08C01B32/05
Inventor 黄世俊罗尧森荀瑞芝童跃进郑方华罗建峰
Owner 沙县宏盛塑料有限公司
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