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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 the problems of slowing down the reaction speed, difficult to achieve satisfactory treatment effect, and affecting product preservation, so as to avoid the generation of waste water and benefit the environment The effect of protection and good economic benefits

Active Publication Date: 2013-12-25
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] Example 1: Preparation of thermoplastic barium sulfate phenolic resin

[0029] The formulation of thermoplastic barium sulfate phenolic resin can be in the following range:

[0030]

[0031] Start the stirring of the 1000-liter reactor with condenser, stirrer, quick opening, jacket steam heating and water cooling, add 250Kg of phenol, 65Kg of solid formaldehyde, 250Kg of polycondensation dehydration fraction or deionized water, and turn on steam to heat to 50-80 After depolymerization of formaldehyde, 1Kg of sulfuric acid (50%) was slowly added, and the temperature was raised to reflux carefully. After the reaction was stable, 2Kg of remaining sulfuric acid (50%) was slowly added in two batches, and the sample was refluxed for 1 hour. The sample was collected at 20 ℃ When the water is not sticky and the hand is hard, the jacket is cooled to the material temperature of 96 ℃, and barium hydroxide (Ba(OH)) is slowly added. 2 *8H 2 0) 4.8Kg neutralize sulfuric acid, st...

Embodiment 2

[0032] Example 2: Preparation of low cardanol thermoplastic barium sulfate phenolic resin

[0033] Recipes can range from:

[0034]

[0035] Start the stirring of the 1000-liter reactor with condenser, stirrer, quick opening, jacket steam heating and water cooling, add 345Kg of phenol, 91Kg of solid formaldehyde, 59Kg of cardanol, and 345Kg of polycondensation dehydration fraction, and open the steam to heat to 50-80 After depolymerization of formaldehyde, 2.3Kg of sulfuric acid (50%) was slowly added, and the temperature was raised to reflux carefully. After the reaction was gentle, the remaining sulfuric acid (50%) 5.4.Kg was slowly added in two steps, and then refluxed for 1 hour and sampled. When the sample does not stick to the hand in 20°C water, the jacket is cooled to a material temperature of 95-96°C, and barium hydroxide (Ba(OH)) is slowly added. 2 *8H 2 O) 12.4Kg neutralize sulfuric acid, terminate catalytic reaction, generate barium sulfate precipitation and w...

Embodiment 3

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

[0037] Recipes can range from:

[0038]

[0039] Start the stirring of the 1000-liter reactor with condenser, stirrer, quick opening, jacket steam heating and water cooling, add 220Kg of phenol, 65Kg of solid formaldehyde, 72Kg of cardanol, polycondensation dehydration fraction and 220Kg of deionized water, turn on steam heating After depolymerizing the formaldehyde at 50~80℃, slowly add 2Kg of sulfuric acid (50%), and carefully heat up to reflux. After the reaction is flat, slowly add 6Kg of remaining sulfuric acid (50%) in two steps and reflux for 1 hour. , the sample is not sticky in water at 20°C and when the jacket is hard, the jacket is cooled to the material temperature of 96°C, and barium hydroxide (Ba(OH)) is slowly added. 2 *8H 20) 4.8Kg neutralize sulfuric acid, stop catalytic reaction, generate barium sulfate precipitation and water, then carry out vacuum dehydration w...

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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, in particular to a process for cyclically 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 adhesives Agents and matrix materials are widely used in military, aviation, aerospace and other cutting-edge technology fields. [0003] Thermoplastic phenolic resin is traditionally produced by polycondensation of phenol and formaldehyde solution under acidic catalyst. Take the production method of thermoplastic phenolic resin c...

Claims

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Application Information

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Patent Type & Authority Applications(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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