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A kind of production method of resorcinol formaldehyde resin

A resorcinol formaldehyde resin and resorcinol technology, applied in the field of resorcinol formaldehyde resin production, can solve the problems of long reaction cycle, long time, high energy consumption, etc., achieve good adhesion performance and avoid environmental pollution , the effect of improving production efficiency

Active Publication Date: 2015-08-26
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since it is a two-step reaction, and each step takes a long time, the disadvantages of long reaction cycle and high energy consumption are also obvious in industrial production.

Method used

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  • A kind of production method of resorcinol formaldehyde resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 500mL five-necked round-bottomed reaction flask equipped with a stirrer, reflux condenser and dropping funnel, add 110.0g (1mol) resorcinol and 2.4g composite catalyst, the mass ratio of oxalic acid and p-toluenesulfonic acid in the composite catalyst =1:9, heat to 110-120°C to melt, then quickly dropwise add 41.7g (0.4mol) styrene and 11.9g (0.15mol) formaldehyde aqueous solution within 20-30 minutes, keep warm and reflux for about 10 minutes, then The process maintains a temperature not higher than 130°C. Then add 10.4g (0.1mol) styrene and 39.5g (0.5mol) formaldehyde solution dropwise within 1 to 1.5 hours, keep warm and reflux for about 15 minutes, and keep the temperature not higher than 120°C during this process. Add 1.75g ​​of sodium hydroxide solution to neutralize the composite catalyst, then stop stirring, wait for the organic phase and the water phase to separate, and extract the upper water phase. Finally, the temperature is raised to 125-150°C, and th...

Embodiment 2

[0033]In a 500mL five-necked round-bottomed reaction flask equipped with a stirrer, reflux condenser and dropping funnel, add 110.0g (1mol) resorcinol and 2.4g composite catalyst, the mass ratio of oxalic acid and p-toluenesulfonic acid in the composite catalyst =1:9, heat to 110-120°C to melt, then add 62.4g (0.6mol) styrene and 11.9g (0.15mol) formaldehyde solution dropwise quickly within 20-30 minutes, keep warm and reflux for about 10 minutes, then The process maintains a temperature not higher than 130°C. Then add 10.4g (0.1mol) styrene and 43.4g (0.55mol) formaldehyde solution dropwise within 1 to 1.5 hours, keep warm and reflux for about 15 minutes, and keep the temperature not higher than 120°C during this process. Add 1.75g ​​of sodium hydroxide solution to neutralize the composite catalyst, then stop stirring, wait until the organic phase and the water phase are separated, extract the upper water phase, and finally raise the temperature to 125-150°C, distill under re...

Embodiment 3

[0035] In a 500mL five-necked round-bottom reaction flask equipped with a stirrer, reflux condenser and dropping funnel, add 220.0g (2mol) resorcinol and 4.8g composite catalyst, the mass ratio of oxalic acid and p-toluenesulfonic acid in the composite catalyst =1:7.5, heat to 110-120°C to melt, then quickly dropwise add an aqueous solution of 104.1g (1mol) styrene and 15.7g (0.2mol) formaldehyde within 20-30 minutes, keep warm and reflux for about 10 minutes, this process Keep the temperature not higher than 130°C. Then add 62.4g (0.6mol) styrene and 47.2g (0.6mol) formaldehyde solution dropwise within 1 to 1.5 hours, keep the temperature under reflux for about 15 minutes, and keep the temperature not higher than 120°C during this process. Add 1.8g of sodium hydroxide solution to neutralize the composite catalyst, then stop stirring, wait until the organic phase and the water phase are separated, take out the upper water phase, and finally raise the temperature to 125-150°C, ...

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Abstract

The invention relates to a production method of resorcinol formaldehyde resin. The method comprises the following steps of: using resorcinol and formaldehyde as raw material, adding the modifier, namely vinyl benzene, performing two-stage polymerization in the presence of composite acid catalyst, firstly, heating the resorcinol and the composite acid catalyst to melt, then, dropping 50%-80% of the modifier and 10%-30% of the formaldehyde into the molten liquid to perform primary polymerization, simultaneously dropping the rest of modifier and the rest of formaldehyde into the primarily polymerized solution to perform main polymerization, and finally, separating out the resorcinol / formaldehyde resin from the polymerization solution. The modified resorcinol formaldehyde resin prepared by the invention is low in the content of free resorcinol, low in smoke development and excellent in adhesive property, and is green and environment-friendly when being used for industrial production.

Description

technical field [0001] The invention relates to the technical field of rubber additive production, in particular to a method for producing resorcinol formaldehyde resin. Background technique [0002] In the production of rubber products, steel cords are often used to enhance the strength of rubber products, and the adhesion between steel cords and rubber will directly affect the service life of rubber products. In the field of automobile tires, rubber and steel wire form a good mechanical bond during vulcanization to obtain excellent initial adhesion, but due to aging and use, the bonding performance weakens and the bond fails prematurely. To avoid this, an adhesion promoter is usually added to maintain the adhesion of the rubber to the steel cord. [0003] In order to promote the adhesion between rubber and steel cord, the traditional method is to add methylene acceptor and methylene donor system before rubber vulcanization. In the early days, resorcinol was used as the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/30C08L7/00C08L61/14
Inventor 杜孟成韩涛宋彦哲
Owner SHANDONG YANGGU HUATAI CHEM