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Preparation Technology of Phenolic Resin Beads with Narrow Diameter Distribution

A technology of phenolic resin and ball diameter, which is applied in the field of preparation of phenolic resin pellets, can solve the problems of high cost, narrow distribution of ball diameters, complicated processes, etc., and achieve the effects of low cost, uniform ball diameter, and controllable ball diameter.

Active Publication Date: 2015-10-28
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese invention patent 99110071 "a method for preparing spherical activated carbon by adding a pore-forming agent" and 98118911 "a method for preparing spherical activated carbon based on mesoporous phenolic resin" are obtained by evaporating the ethanol solution of phenolic resin to remove the solvent. For pelletized phenolic resin particles, although the ball diameter is easy to control and the ball diameter distribution is narrow, the biggest problem of this method is that the reproducibility is poor during evaporation and desolventization, and the process is complicated, poor controllability, and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Add hexamethylenetetramine into the phenolic resin powder at 1% of the mass of the phenolic resin, mix well, put it into the mold at a rate of 0.5°C / min to 120°C and keep the temperature constant for 0.5h, then press 200kg / min cm 2 The pressure molding extruded strip with a diameter of 2mm; the strip was added to an autoclave containing a concentration of 1wt% polyvinyl alcohol aqueous solution (the quality of polyvinyl alcohol was 1% of the phenolic resin), and the temperature was closed and heated. At a stirring speed of 200 rpm, the temperature was raised to 120 °C at a rate of 0.5 °C / min and kept at a constant temperature for 5 hours. After cooling down, the solid and liquid were separated, and 92% of phenolic resin pellets with a diameter of 1.8-2.0 mm were obtained.

Embodiment 2

[0019] Hexamethylenetetramine was added to the phenolic resin powder at 15% of the mass of the phenolic resin, and after being thoroughly mixed, it was placed in a mold and raised to 80°C at a heating rate of 1°C / min and kept at a constant temperature for 2 hours, and then pressed at a rate of 450kg / cm2 Pressure molding extrudes a strip with a diameter of 0.4mm; add the strip to an aqueous solution containing 5wt% sodium octadecylsulfonate (the quality of sodium octadecylsulfonate is 10% of the phenolic resin) In the autoclave, heat up in a closed manner, raise the temperature to 160°C at a rate of 1°C / min at a stirring speed of 600 rpm and keep the temperature constant for 1 hour. After cooling down, the solid and liquid are separated to obtain 90% of phenolic formaldehyde with a spherical diameter of 0.3-0.4mm Resin pellets.

Embodiment 3

[0021] Add hexamethylenetetramine into the phenolic resin powder according to 10% of the mass of the phenolic resin, mix thoroughly and evenly, and then add it into the screw extruder. ℃, the third section is 80°C, and the fourth section is 100°C. After staying in the extruder for 1h, a strip with a diameter of 2mm is obtained; the strip is added to a concentration of 2wt% dodecyl In the autoclave of sodium sulfate aqueous solution (the mass of sodium lauryl sulfate is 4% of the phenolic resin), heat up in a closed manner, raise the temperature to 130°C at a stirring speed of 400 rpm at a rate of 0.8°C / min and keep the temperature constant for 2 hours , solid-liquid separation after cooling down to obtain 95% of phenolic resin pellets with a diameter of 1.9-2.0mm.

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Abstract

The invention discloses a preparation technology of a phenolic resin sphere with narrow sphere diameter distribution. The preparation technology is characterized by comprising the steps of adding hexamethylene tetramine into phenolic resin powder, mixing uniformly, and then, extruding to form a stripe; preparing a water solution of a dispersing agent with the concentration of 1-5wt%, wherein the mass of the dispersing agent accounts for 1-10% of the phenolic resin; directly adding the water solution of the dispersing agent and the stripe into a high-pressure kettle, sealing, heating to 120-160 DEG C while stirring at a certain rotating speed, and preserving the constant temperature for 1-5h; carrying out solid-liquid separation after cooling to obtain the phenolic resin sphere with narrow sphere diameter distribution. The preparation technology has the advantages of low cost, good repeatability and narrow sphere diameter distribution.

Description

technical field [0001] The invention belongs to a preparation technology of phenolic resin balls, in particular to a preparation technology of phenolic resin balls with narrow ball diameter distribution. Background technique [0002] Due to its high carbon residue rate and its ability to deform and shrink into a spherical shape at a certain temperature, thermoplastic phenolic resin can be prepared into a spherical resin to expand its application range. [0003] Chinese invention patents 200410012346 "a preparation method of phenolic resin-based microspheres", 200810079389 "a preparation method of spherical phenolic resin", 200410016702 "a preparation method of porous phenolic resin-based carbon microspheres" and so on all use phenolic resin Although the ethanol solution is used to form balls, although the operation is simple, the obtained phenolic resin balls have a wide distribution of ball diameters, and it is necessary to classify by sieving to obtain small balls with bas...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J3/12C08L61/06
Inventor 李开喜
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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