Phenolic resin for environment-friendly thermoplastic refractory material and preparation method thereof

Abstract

The invention relates to phenolic resin for an environment-friendly thermoplastic refractory material and a preparation method thereof, and the material comprises the following components: 100 parts of phenol, 20-25 parts of solid paraformaldehyde, 0.2-0.4 part of acid catalyst, 0.2-2.0 part of alkaline solution and 20-30 parts of solvent. The phenol and the acid catalyst are added into a reactor, the temperature is raised to 90 DEG C, then all the solid paraformaldehyde is slowly and completely added into the reactor within 2.5-3.5 hours, and the solution temperature is controlled to be 90-108 DEG C; after the solid paraformaldehyde is added completely, the solution temperature is controlled to be 95-110 DEG C, and then the constant temperature is kept for 3-4 hours for performing phenolic aldehyde polycondensation reaction; after the reaction is finished, the alkaline solution is further added into the solution, and the pH value of the solution is regulated to 6.5-7.5; and a solventis simultaneously added into the solution, and the phenolic resin for the refractory material is finally obtained. The production process is safe and reliable, vacuum dehydration is unnecessary, sewage discharge can be avoided, an ecological environment can be protected, and the production efficiency can be improved.

Description

Technical field:

[0001] The invention relates to a phenolic resin and a preparation method thereof, in particular to an environment-friendly phenolic resin for thermoplastic refractory materials and a preparation method thereof. Background technique:

[0002] Phenolic resin for refractory materials, due to its high residual carbon rate and good wettability to refractory aggregates and graphite, the mud can be mixed and formed at room temperature. After drying, the phenolic resin will be carbonized Forming a continuous bonded carbon skeleton can improve the strength and corrosion resistance of carbon composite refractories.

[0003] In the past, phenolic resin was obtained by the polycondensation reaction of phenol and formaldehyde solution. During the synthesis process, phenol and formaldehyde solution were sequentially added to the reactor equipped with a stirrer, reflux condenser, thermometer, steam heating interlayer and vacuum device. Stir at a constant speed and heat u...

Examples

Embodiment 1

[0021] Example 1: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 25 parts of solid paraformaldehyde, 0.4 parts of hydrochloric acid, 0.25 parts of ammonia water, 17 parts of ethylene glycol, and 8 parts of ethanol.

[0022] Its preparation method comprises the following steps:

[0023] (1), in the reactor that agitator, reflux condenser and thermometer are housed, add 100 parts of molten phenol, add concentration simultaneously and be 0.3 part of hydrochloric acid of 36%, heat while stirring;

[0024] (2), when the temperature of the solution of phenol and hydrochloric acid rose to 90°C, slowly add 24 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 3.5 hours. In the process of adding, control the temperature of the solution in the reactor between 90~108°C;

[0025] (3), after solid paraformaldehyde has been added, control the tempe...

Embodiment 2

[0027] Example 2: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 23.5 parts of solid paraformaldehyde, 0.37 parts of sulfuric acid, 2 parts of triethanolamine, 20 parts of ethylene glycol, and 4 parts of methanol.

[0028] Its preparation method comprises the following steps:

[0029] (1), in the reactor that agitator, reflux condenser and thermometer are equipped with, add 100 parts of molten phenols, add concentration simultaneously and be 0.37 parts of sulfuric acid of 20%, heat while stirring;

[0030] (2), when the temperature of the solution of phenol and sulfuric acid rose to 90°C, start to slowly add 23.5 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 3 hours. During the addition process, the temperature of the solution in the control reactor is between 90~105°C;

[0031] (3), after solid paraformaldehyde has been added, c...

Embodiment 3

[0033] Example 3: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 24 parts of solid paraformaldehyde, 0.3 parts of hydrochloric acid, 0.3 parts of sodium hydroxide, 17 parts of ethylene glycol, and 3 parts of ethanol.

[0034] Its preparation method comprises the following steps:

[0035] (1), in the reactor that agitator, reflux condenser and thermometer are housed, add 100 parts of molten phenol, add concentration simultaneously and be 0.3 part of hydrochloric acid of 36%, heat while stirring;

[0036] (2), when the temperature of the solution of phenol and hydrochloric acid rose to 90°C, slowly add 24 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 2.8 hours. In the process of adding, control the temperature of the solution in the reactor between 90~108°C;

[0037] (3), after solid paraformaldehyde has added, control the temperat...

Technical field:

[0001] The invention relates to a phenolic resin and a preparation method thereof, in particular to an environment-friendly phenolic resin for thermoplastic refractory materials and a preparation method thereof. Background technique:

[0002] Phenolic resin for refractory materials, due to its high residual carbon rate and good wettability to refractory aggregates and graphite, the mud can be mixed and formed at room temperature. After drying, the phenolic resin will be carbonized Forming a continuous bonded carbon skeleton can improve the strength and corrosion resistance of carbon composite refractories.

[0003] In the past, phenolic resin was obtained by the polycondensation reaction of phenol and formaldehyde solution. During the synthesis process, phenol and formaldehyde solution were sequentially added to the reactor equipped with a stirrer, reflux condenser, thermometer, steam heating interlayer and vacuum device. Stir at a constant speed and heat u...

Examples

Embodiment 1

[0021] Example 1: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 25 parts of solid paraformaldehyde, 0.4 parts of hydrochloric acid, 0.25 parts of ammonia water, 17 parts of ethylene glycol, and 8 parts of ethanol.

[0022] Its preparation method comprises the following steps:

[0023] (1), in the reactor that agitator, reflux condenser and thermometer are housed, add 100 parts of molten phenol, add concentration simultaneously and be 0.3 part of hydrochloric acid of 36%, heat while stirring;

[0024] (2), when the temperature of the solution of phenol and hydrochloric acid rose to 90°C, slowly add 24 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 3.5 hours. In the process of adding, control the temperature of the solution in the reactor between 90~108°C;

[0025] (3), after solid paraformaldehyde has been added, control the tempe...

Embodiment 2

[0027] Example 2: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 23.5 parts of solid paraformaldehyde, 0.37 parts of sulfuric acid, 2 parts of triethanolamine, 20 parts of ethylene glycol, and 4 parts of methanol.

[0028] Its preparation method comprises the following steps:

[0029] (1), in the reactor that agitator, reflux condenser and thermometer are equipped with, add 100 parts of molten phenols, add concentration simultaneously and be 0.37 parts of sulfuric acid of 20%, heat while stirring;

[0030] (2), when the temperature of the solution of phenol and sulfuric acid rose to 90°C, start to slowly add 23.5 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 3 hours. During the addition process, the temperature of the solution in the control reactor is between 90~105°C;

[0031] (3), after solid paraformaldehyde has been added, c...

Embodiment 3

[0033] Example 3: An environment-friendly phenolic resin for thermoplastic refractory materials, the material components are 100 parts of phenol, 24 parts of solid paraformaldehyde, 0.3 parts of hydrochloric acid, 0.3 parts of sodium hydroxide, 17 parts of ethylene glycol, and 3 parts of ethanol.

[0034] Its preparation method comprises the following steps:

[0035] (1), in the reactor that agitator, reflux condenser and thermometer are housed, add 100 parts of molten phenol, add concentration simultaneously and be 0.3 part of hydrochloric acid of 36%, heat while stirring;

[0036] (2), when the temperature of the solution of phenol and hydrochloric acid rose to 90°C, slowly add 24 parts of solid paraformaldehyde to the above solution, and the solid paraformaldehyde should be controlled within 2.8 hours. In the process of adding, control the temperature of the solution in the reactor between 90~108°C;

[0037] (3), after solid paraformaldehyde has added, control the temperat...