A kind of preparation method of phenolic resin for refractory material

A technology of phenolic resin and refractory materials, applied in the field of refractory materials, can solve the problems of excessive formaldehyde concentration, environmental re-pollution, explosion, etc., and achieve the effect of improving product yield and improving compressive strength

Active Publication Date: 2021-03-02
JINAN LUDONG REFRACTORY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The above-mentioned original process adopts the method of slowly adding solid paraformaldehyde to the solution of phenol and acidic catalyst. Although this method can successfully prepare the phenolic resin for environment-friendly thermoplastic refractory materials, it has the following disadvantages: in the later stage of the reaction, the solid paraformaldehyde will After being added into the container, the solid paraformaldehyde with larger particles will form a layer of film on the surface, resulting in the inability of depolymerization and condensation reaction of the solid paraformaldehyde, which affects the product quality and resin yield
Moreover, when the resin containing unreacted solid paraformaldehyde is used as a refractory material, free formaldehyde is precipitated during the high-temperature drying process, resulting in excessive formaldehyde concentration in the drying tunnel kiln, causing explosion hazards in severe cases, and causing environmental pollution again.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Phenol 1000kg, solid paraformaldehyde 238kg, hydrochloric acid 3.6kg, ethanol ethylene glycol mixed solvent 320kg.

[0030] Preparation steps:

[0031] (1) Depolymerization and fusion reaction: Put solid paraformaldehyde and phenol into a closed container, turn on the stirring and container water circulation condensation system and heat up to 100°C to 130°C to completely depolymerize the solid paraformaldehyde and Dissolve in phenol solution, stop heating and stirring, wait until it is cooled to 50°C-90°C, close the water circulation condensing system, and dissolve the solution for use.

[0032] (2) Condensation reaction: slowly inject the fusion solution in step 1 into the reactor through the reactor liquid flow rate control device, and the injection flow rate is controlled at 15-25kg / min, and at the same time, slowly inject the catalyst into the reactor through another flow rate controller, and inject The flow rate is 50-70g / min, and the two liquids are put in at the...

Embodiment 2

[0035] Phenol 1000kg, solid paraformaldehyde 200kg, 20% sulfuric acid 3.7kg, alkaline solution (99% triethanolamine) 20kg, diluent 340kg.

[0036] Preparation steps:

[0037] (1) Depolymerization and fusion reaction: Put solid paraformaldehyde and phenol into a closed container, turn on the stirring and container water circulation condensation system and heat up to 100°C to 130°C to completely depolymerize the solid paraformaldehyde and Dissolve in phenol solution, stop heating and stirring, wait until it is cooled to 50°C-90°C, close the water circulation condensing system, and dissolve the solution for use.

[0038](2) Condensation reaction: the fusion solution in step 1 is slowly injected into the reactor through the reactor liquid flow rate control device, and the flow rate is controlled at 15 to 25 kg / min. At the same time, the catalyst is slowly injected into the reactor through another flow rate controller, and the flow rate is 50-70g / min, the two liquids are put in at...

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Abstract

The invention provides a preparation method of phenolic resin for a fireproof material. The preparation method comprises the following preparation steps: (1) depolymerization and solvation reaction: adding solid paraformaldehyde and phenol into a sealed container; enabling the solid paraformaldehyde to be completely depolymerized and dissolved into a phenol solution to obtain a solvated solution for later use; (2) condensation reaction: slowly injecting the solvated solution in step 1 into a reactor; meanwhile, slowly injecting a catalyst into the reactor, simultaneously adding two types of liquid according to the quantity ratio and stirring at a low speed; after injecting two types of solutions, continually keeping reaction time for 60 to 80 minutes; (3) adjusting the viscosity and canning: cooling the phenolic resin reacted in step 2; adding the diluting agent and adjusting the viscosity and canning. The mol ratio of the phenol to the solid paraformaldehyde is 1 to (0.5 to 0.9). Themethod provided by the invention ensures that the solid paraformaldehyde reacts completely and has no residues; the safety and environment pollution problems of a former technology are solved and thecompressive strength of the fireproof material is improved.

Description

technical field [0001] The invention relates to a preparation method of phenolic resin for refractory materials, belonging to the technical field of refractory materials. Background technique [0002] The applicant ZL 2011100063565.8, in the patent titled a phenolic resin for environmentally friendly thermoplastic refractory materials and its preparation method, provides an environmentally friendly phenolic resin for thermoplastic refractory materials and its preparation method, the material component of which is phenol 100 20-25 parts of solid paraformaldehyde, 0.2-0.4 parts of acid catalyst, 0.2-2.0 parts of alkaline solution, and 20-30 parts of solvent. Add phenol and acidic catalyst to the reactor, raise the temperature to 90°C, then slowly add all the solid paraformaldehyde to the reactor within 2.5 to 3.5 hours, and control the solution temperature between 90 and 108°C; solid paraformaldehyde After adding, control the temperature of the solution between 95-110°C, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10
CPCC08G8/10
Inventor 刘在春吕仁祥宋方平
Owner JINAN LUDONG REFRACTORY CO LTD
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