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A kind of preparation method of phenolic resin microsphere

A technology of phenolic resin and resole phenolic resin, which is applied in the field of preparation of phenolic resin microspheres, can solve the problems of increasing operation steps, difficult sphericity, and wide particle size distribution of microspheres, and achieves the effect of reducing costs and simple steps

Active Publication Date: 2018-11-30
昆山昆鹏利杰高分子材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of operation is simple, but the disadvantage is that it is necessary to disperse the phenolic resin in ethanol or methanol, which increases the operation steps, and the phenolic resin microspheres are suspended in the mixed oil of heat transfer oil and silicone oil, which makes solid-liquid separation difficult. , the degree of sphericity is difficult to control, and the particle size distribution of microspheres is wide

Method used

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  • A kind of preparation method of phenolic resin microsphere
  • A kind of preparation method of phenolic resin microsphere
  • A kind of preparation method of phenolic resin microsphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put commercial resole phenolic resin, sodium lauryl sulfate, and methyl silicone oil directly into the container at a mass ratio of 1:0.09:9.4, stir at a constant speed of 800 rpm, raise the temperature to 130°C, and keep the temperature constant for 1h , adding oxalic acid, adjusting the pH value of the solution to 0.4, and keeping the temperature at a constant temperature for 1 h, pouring out the upper layer of methyl silicone oil, washing, and drying to obtain spherical phenolic resin particles. The average particle size of the phenolic resin microspheres obtained by the method is about 20 μm, the particle size is uniform, and the sphericity is good.

Embodiment 2

[0027] Put commercial resole phenolic resin, sodium lauryl sulfate, and paraffin oil directly into the container at a mass ratio of 1:0.05:7.5, stir at a constant speed of 550 rpm, raise the temperature to 130°C, and keep the temperature constant for 1h. Add hydrochloric acid to adjust the pH value of the solution to 0.4, and keep the temperature constant for 1 hour, pour out the paraffin oil in the upper layer, wash and dry to obtain spherical phenolic resin particles. The average particle size of the phenolic resin microspheres obtained by the method is between 50-100 μm, the particle size is uniform, and the sphericity is good.

Embodiment 3

[0029] Put commercial resole phenolic resin, sodium lauryl sulfate, and methyl silicone oil directly into the container at a mass ratio of 10:0.5:20, stir at a constant speed of 800 rpm, heat up to 150°C, and keep the temperature constant for 1h , adding citric acid, adjusting the pH value of the solution to 0.4, and keeping the temperature constant for 2 hours, pouring out the upper layer of methyl silicone oil, washing and drying to obtain spherical phenolic resin particles. The average particle size of the phenolic resin microspheres obtained by the method is between 300-500 μm, the particle size is uniform, and the sphericity is good.

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Abstract

The invention aims at providing a preparation method of phenolic resin microspheres, which is simple, convenient to operate, and relatively low in production costs. The preparation method concretely comprises the steps of adding commercial resol, a surface active agent and a dispersion liquid into a reaction vessel at the mass ratio of (0.05 to 10):(0.05 to 2.5):(5 to 50), keeping a certain stirring speed, and heating to react for a certain period of time; adjusting the pH value by adding acidoid, performing thermostatic reaction for a certain period of time, separating out the phenolic resin microspheres from a solvent, pouring out supernatant, and obtaining the spherical phenolic resin microspheres by washing and drying. According to the method, the step of evenly mixing phenolic resin in ethyl alcohol or methyl alcohol is omitted; the dispersion liquid subjected to separation can be recycled; the costs are favorably reduced; and the size distribution of the obtained phenolic resin microspheres is relatively uniform.

Description

technical field [0001] The invention relates to the technical field of composite materials, in particular to a preparation method of phenolic resin microspheres. Background technique [0002] There are many methods for preparing phenolic resin microspheres, but these methods are expensive to prepare, and the preparation process is complex and time-consuming. In the patent "Preparation Method of Phenolic Resin-Based Microspheres" with the publication number CN1583837A, the operation steps are as follows: first mix novolac resin with hexamethylenetetramine and dissolve them in methanol / ethanol to form a phenolic resin alcohol solution ; Then the surfactant and water are made into an aqueous solution containing the surfactant; then the phenolic resin alcohol solution is added to the aqueous solution containing the surfactant, and stirred at a constant speed and heated to 110-200°C and kept at a constant temperature for 30-180min to obtain a spherical Phenolic Resin. Although ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/16C08L61/06
CPCC08J3/16C08J2361/06C08L61/06
Inventor 王安苗徐婷婷刘杰万青李伟王然
Owner 昆山昆鹏利杰高分子材料技术有限公司
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