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Process for circularly producing thermoplastic barium sulfate phenolic resin by precipitation method

A technology of phenolic resin and barium sulfate, which is applied in the field of cyclic production of thermoplastic barium sulfate phenolic resin by precipitation method, can solve problems such as difficult to achieve satisfactory treatment effect, slow down reaction speed, affect product preservation, etc., and achieve environmental protection and avoid waste water produce good economic benefits

Active Publication Date: 2015-05-13
计菁婕 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The above method has the following disadvantages: (1) A large amount of waste water will be produced in the production process of the washing process, and two tons of waste water will be produced for every ton of phenolic resin produced. The waste water contains hydrochloric acid, free phenol, lost resin and phenolic derivatives, and the treatment contains Cl ˉ , Phenol-containing wastewater is difficult and expensive, and requires a lot of manpower, equipment and funds, and the treatment effect is difficult to achieve satisfactory results, which will cause great pollution to the environment
(2) The water washing process cannot completely terminate the catalytic reaction, but only slows down the reaction speed
The resin is easy to lose during washing, and the lost resin can only be made into a low-priced low-molecular-weight resin during wastewater treatment
(3) A small amount of Cl contained in the resin ˉ Ions will affect product preservation and easily discolor the resin
[0005] Due to the low utilization rate of raw materials in the traditional washing process of thermoplastic phenolic resin, high production cost per unit output, low yield, large waste, short storage period, large power consumption, large water consumption, large area occupied by wastewater treatment, and high cost, it has seriously hindered Development of phenolic industry

Method used

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  • Process for circularly producing thermoplastic barium sulfate phenolic resin by precipitation method
  • Process for circularly producing thermoplastic barium sulfate phenolic resin by precipitation method
  • Process for circularly producing thermoplastic barium sulfate phenolic resin by precipitation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: prepare thermoplastic barium sulfate phenolic resin

[0029] Preparation of thermoplastic barium sulfate phenolic resin formula can be in the following ranges:

[0030]

[0031] Start the stirring of a 1000-liter reactor with condenser, agitator, quick opening, jacketed steam heating and water cooling, add 250Kg of phenol, 65Kg of solid formaldehyde, 250Kg of polycondensation dehydration fraction or deionized water, and heat to 50-80 After the formaldehyde is depolymerized at ℃, slowly add 1Kg of sulfuric acid (50%), and carefully raise the temperature to reflux. After the reaction is gentle, slowly add the remaining 2Kg of sulfuric acid (50%) and then reflux for 1 hour to sample. The sample is at 20 When the water is not sticky and hard, the jacket is cooled to a material temperature of 96°C, and barium hydroxide (Ba(OH) 2 *8H 2 O) 4.8Kg neutralizes sulfuric acid, terminates the catalytic reaction, generates barium sulfate precipitate and water, then...

Embodiment 2

[0032] Embodiment 2: the preparation of low cardanol thermoplastic barium sulfate phenolic resin

[0033] Recipes can be in the following ranges:

[0034]

[0035] Start the stirring of a 1000-liter reactor with condenser, agitator, quick opening, jacketed steam heating and water cooling, add 345Kg of phenol, 91Kg of solid formaldehyde, 59Kg of cardanol, 345Kg of polycondensation dehydration fraction, and heat to 50-80 After the formaldehyde is depolymerized at ℃, slowly add 2.3Kg of sulfuric acid (50%), and carefully raise the temperature to reflux. After the reaction is gentle, slowly add the remaining 5.4.Kg of sulfuric acid (50%) in two times and then reflux for 1 hour to sample. When the sample is not sticky and hard in 20°C water, the jacket is cooled to a material temperature of 95-96°C, and barium hydroxide (Ba(OH)) is added slowly. 2 *8H 2 O) 12.4Kg neutralizes sulfuric acid, terminates the catalytic reaction, generates barium sulfate precipitate and water, and t...

Embodiment 3

[0036] Embodiment 3. Preparation of high cardanol thermoplastic barium sulfate phenolic resin

[0037] Recipes can be in the following ranges:

[0038]

[0039] Start the stirring of a 1000-liter reactor with condenser, agitator, quick opening, jacketed steam heating and water cooling, add 220Kg of phenol, 65Kg of solid formaldehyde, 72Kg of cardanol, polycondensation dehydration fraction and 220Kg of deionized water, and turn on steam heating After the formaldehyde is depolymerized at 50-80°C, slowly add 2Kg of sulfuric acid (50%), and carefully raise the temperature to reflux. After the reaction is gentle, slowly add the remaining 6Kg of sulfuric acid (50%) in two times and then reflux for 1 hour to sample , when the sample is not sticky and hard in 20°C water, the jacket is cooled to a material temperature of 96°C, and barium hydroxide (Ba(OH) 2 *8H 2O) 4.8Kg neutralizes sulfuric acid, terminates the catalytic reaction, generates barium sulfate precipitate and water, a...

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Abstract

The invention provides a process for circularly producing thermoplastic barium sulfate phenolic resin by a precipitation method. The process comprises the following steps: according to a formula of synthetic resin, adding phenol, solid aldehyde and water into a reaction kettle with a cooler and a stirrer, heating to a temperature of 50 to 80 DEG C, depolymerizing and adding sulfuric acid to perform the catalytic reaction until a sampled sample is not sticky and is slightly hard in water with a temperature of 20 DEG C; cooling a reaction material to a temperature of 95 to 96 DEG C and adding barium hydroxide with stirring to stop the catalytic reaction; neutralizing the sulfuric acid by the barium hydroxide to generate water and barium sulfate precipitates, enabling the pH value of the reaction material to be 7, firstly carrying out normal pressure processing and then carrying out vacuum dehydration to obtain the semitransparent solid thermoplastic barium sulfate phenolic resin product and a polycondensation dehydration fraction; reusing the polycondensation dehydration fraction into the reaction kettle to carry out circular production. The process has zero discharge of wastewater, is beneficial to the environment protection, is suitable for industrial production and has good economic benefits.

Description

technical field [0001] The invention belongs to the field of phenolic resin synthesis, and in particular relates to a process for circularly producing thermoplastic barium sulfate phenolic resin by a precipitation method, which can achieve zero discharge of waste water and almost 100% utilization rate of raw material phenol. Background technique [0002] Thermoplastic phenolic resin products are mainly used in wood bonding processing, molding compounds, insulating materials, heat and sound insulation materials, friction materials, coatings, inks, oil fields, paints, rubber and other industries, among which modified phenolic resins are used as high temperature resistant adhesives Agents and matrix materials are widely used in military, aviation, aerospace and other cutting-edge technology fields. [0003] The traditional production of thermoplastic phenolic resin is made by polycondensation reaction of phenol and formaldehyde aqueous solution under the acidic catalyst. Takin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/10C08G8/28C08K3/30C08L61/10C08L61/14
Inventor 计菁婕计卫国王风
Owner 计菁婕
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