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Preparation method of phenolic resin polymer microspheres

A technology of phenolic resin and polymer, which is applied in the field of preparing spherical phenolic resin polymer by one-pot one-step method, which can solve the problems of difficult control of particle size, high labor intensity, poor sphericity, etc., and achieve uniform particle size distribution, surface Smooth, highly spherical effect

Inactive Publication Date: 2010-01-13
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above two methods for preparing spherical phenolic resins, the former is difficult to control the particle size, labor-intensive, and poor in sphericity
The latter requires a multi-step reaction, the reaction cycle is long, and the ball forming process is cumbersome

Method used

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  • Preparation method of phenolic resin polymer microspheres
  • Preparation method of phenolic resin polymer microspheres
  • Preparation method of phenolic resin polymer microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Example 1: 0.5 g of hydroxypropyl methylcellulose, 27.74 g of ethylene glycol monophenyl ether, 61.00 g of formic acid, and 70.42 g of formaldehyde were mixed uniformly, and then 14.67 g of concentrated sulfuric acid was slowly added dropwise at room temperature. After the dropwise addition, heat to 70 degrees Celsius and stir for 6 hours; filter out the polymer microspheres, soak the solution with 5% sodium hydroxide for 5 hours, wash with water until neutral, and dry.

[0013] The scanning electron micrograph of gained phenolic resin type polymer microsphere is as follows figure 1 shown.

Embodiment 2

[0014] Example 2: 2.59 grams of hydroxypropyl methylcellulose, 27.74 grams of ethylene glycol monophenyl ether, 61.00 grams of formic acid, and 70.42 grams of formaldehyde were mixed uniformly, and then 14.67 grams of concentrated sulfuric acid was slowly added dropwise at room temperature. After the dropwise addition, heat to 70 degrees Celsius and stir for 6 hours; filter out the polymer microspheres, soak the solution with 5% sodium hydroxide for 5 hours, wash with water until neutral, and dry.

[0015] Gained phenolic resin type polymer microsphere particle size distribution is as follows Figure 4 shown.

Embodiment 3

[0016] Example 3: 0.79 g of carboxymethylmethyl cellulose, 27.74 g of ethylene glycol monophenyl ether, 61.00 g of formic acid, and 35.55 g of formaldehyde were mixed uniformly, and then 14.67 g of concentrated sulfuric acid was slowly added dropwise at room temperature. After the dropwise addition, it was heated to 70 degrees Celsius and stirred for 6 hours; the polymer microspheres were filtered out, soaked in 5% sodium hydroxide solution for 5 hours, washed with water until neutral, and dried.

[0017] The scanning electron micrograph of gained phenolic resin type polymer microsphere is as follows figure 2 shown.

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Abstract

The invention discloses a preparation method of phenolic resin polymer microspheres. The method overcomes the defect that the former preparation method adopts a single stabilizer and can adopt different stabilizers as required to prepare phenolic microspheres of different grain diameter distributions to obtain a globular polymer with smooth surface and uniform grain fineness distribution. The method includes the steps of uniformly mixing stabilizer hydroxypropyl methyl cellulose (or carboxymethyl cellulose or arabicgum), ethylene glycol monophenyl ether, formic acid and formaldehyde, then slowly dipping concentrated sulfuric acid, after dipping, heating and stirring the reaction mixture under a certain temperature to react for a certain time and drying the product after separating, soaking in alkali solution and washing. The phenolic resin polymer microsphere prepared by the invention achieves high sphericity and the grain diameter ranging from 0.1-1.5mm by one step reaction, can be used as the base material of macromolecule absorbent and is used for the fields of biological medicines, chromatographic separation and environment treatment, etc.

Description

(1) Technical field: [0001] The invention relates to a preparation method of phenolic resin type polymer microspheres, in particular to a method for preparing spherical phenolic resin type polymers through a one-pot, one-step method. (two) background technology: [0002] Phenolic resin first appeared in 1907 and is the first thermosetting resin successfully developed and commercialized in the world. The resin is a high molecular polymer formed by polycondensation reaction of phenol and formaldehyde under the catalysis of acid or alkali. There are usually two polycondensation methods for phenolic resins, that is, condensing excess formaldehyde phenol under the action of a basic catalyst or condensing formaldehyde and excess phenol under the action of an acidic catalyst. In recent years, phenolic resin microspheres have been used in environmental protection, biomedicine, military, chemical industry, analysis, energy storage materials, etc. due to their high mechanical strengt...

Claims

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Application Information

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IPC IPC(8): C08G16/02
Inventor 纪春暖孙言志曲荣君王春华时京喜刘丽
Owner LUDONG UNIVERSITY
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