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Morpholine modified p-tert-butylphenol-formaldehyde resin and preparation method thereof

A technology of p-tert-butyl and phenolic resin, applied in organic chemistry and other directions, can solve the problems of complex production process, high price, explosiveness, etc., and achieve the effects of simple process, convenient operation and low price

Active Publication Date: 2011-12-28
WUHAN JINGHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] For a long time, in order to improve the viscosity and processing performance of rubber and ensure the integrity of products during molding and molding, people have tried to develop different types of tackifiers in different periods, including rosin and its esters, terpene resins , coumarone resin, petroleum resin and alkylphenolic resin, among the above varieties, alkylphenolic resin has the best tackifying effect, and has become the backbone product of tackifier to occupy the market, but this kind of resin does not have excellent storage viscosity and Wet heat viscosity performance, the storage viscosity of the rubber compound added with ordinary resin is 1-3 days, which cannot meet the production needs of high-end tires and rubber products
At present, some high-grade tires use imported super tackifying resin (p-tert-butylphenol-acetylene resin produced by BASF in Germany), and its price is particularly high, reaching 40,000 yuan per ton, and p-tert-butylphenol produced by BASF in Germany - Acetylene resin needs to add acetylene in production, but acetylene is flammable and explosive, and the production process is extremely complicated

Method used

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  • Morpholine modified p-tert-butylphenol-formaldehyde resin and preparation method thereof
  • Morpholine modified p-tert-butylphenol-formaldehyde resin and preparation method thereof
  • Morpholine modified p-tert-butylphenol-formaldehyde resin and preparation method thereof

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preparation example Construction

[0034] The preparation method of morpholine modified p-tert-butylphenol-formaldehyde resin is characterized in that it is made of the following components in an amount by weight: 20-35 parts of morpholine, 300-320 parts of p-tert-butylphenol, the first The first step is 125-130 parts of formaldehyde with a weight content of 37%, 0.3-0.5 parts of catalyst, 1.4-2 parts of sodium bicarbonate, 400-500 parts of toluene, and the second step is 25 parts of formaldehyde with a weight content of 37%, hydrochloric acid Or 2-3 parts of oxalic acid, 0.3 parts of active agent;

[0035] The catalyst is an inorganic acid or an organic acid, and the active agent is a copper ammonium complexing agent;

[0036] The described components are made according to the following steps: (1), put in metered p-tert-butylphenol, heat up to 100°C and stop heating, start stirring after all melting, control the stirring speed to 65-85 rpm, stir for half After 1 hour, add the prepared metered catalyst and act...

Embodiment 1

[0046] Add 300g of p-tert-butylphenol into a 1000mL three-necked flask, raise the temperature to 100°C, stop heating, start stirring after it is completely melted, control the stirring speed at 65 rpm, and add 0.3g of copper ammonium complexing agent that has been prepared. Add 0.35g of catalyst, stir for 30 minutes after adding, stabilize the temperature at 60-95°C, add dropwise 125g of formaldehyde in the first step, keep warm at 65-100°C for 3 hours after adding, after the reaction, add metered hydrogen carbonate Sodium 2g (make 20% aqueous solution according to the mass ratio, neutralize, adjust the pH value to about 7-10, control the temperature at 65-100°C and slowly add 26g of measured morpholine, and continue to add slowly after adding The second step is 25g of formaldehyde (adding in about 45 minutes). After the addition, keep warm at 65-100°C for 1.5 hours. If the material is thicker, add 50g of toluene, and then add 2.6g of 31% hydrochloric acid solution measured by ...

Embodiment 2

[0048] Add 310g of p-tert-butylphenol into a 1000mL three-neck flask, raise the temperature to 100°C and stop heating, start stirring after it is completely melted, control the stirring speed at 85 rpm, and add 0.3g of copper ammonium complexing agent that has been prepared and measured Add 0.5g of catalyst, stir for 30 minutes after adding, stabilize the temperature at 60-95°C, add dropwise 130g of formaldehyde in the first step, keep warm at 65-100°C for 3 hours after adding, after the reaction, add metered amount of hydrogen carbonate Sodium 1.8g (make 20% aqueous solution according to mass ratio, carry out neutralization, adjust pH value to be about 7-10, control temperature at 65-100 ℃ and slowly add metered morpholine 35g, continue to drop slowly after adding Add 25g of formaldehyde in the second step (adding in about 45 minutes), keep warm at 65-100°C for 1.5 hours after adding, if the material is thicker, add 50g of toluene, and then add 2.6g of 31% hydrochloric acid so...

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Abstract

The invention relates to a morpholine modified para-tert-butyl phenolic resin and is characterized in that the structural formula of the morpholine modified para-tert-butyl phenolic resin is described in the specification, wherein R is morpholine, n can be 1,2,3,4 or 5, and the average molecule weight of the substance is 800-1000. According to the invention, the resin can improve the tackifying property of a product so that the tackifying property of the product meets the processing technology of automobile tyre and rubber; and the performance of the resin is equivalent to that of para-tert-butyl phenol-acetylene resin produced by BASF in German. The invention also discloses the preparation process of the morpholine modified para-tert-butyl phenolic resin.

Description

technical field [0001] The invention relates to a morpholine-modified p-tert-butylphenol-formaldehyde resin, and also relates to a preparation method of the morpholine-modified p-tert-butylphenol-formaldehyde resin. Background technique [0002] With the development of the rubber industry, the amount of synthetic rubber is increasing rapidly. In addition, its application fields are expanding day by day, processing technology is constantly improving, and the requirements for rubber adhesion performance are getting higher and higher. People are increasingly aware of the importance of rubber tackifiers. Looking forward to the advent of new and efficient tackifiers. [0003] For a long time, in order to improve the viscosity and processing performance of rubber and ensure the integrity of products during molding and molding, people have tried to develop different types of tackifiers in different periods, including rosin and its esters, terpene resins , coumarone resin, petroleu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/096C08K5/357C08L7/00C08L9/06C08L9/00C08L23/16
Inventor 王腊生严建国刘建兵童凡
Owner WUHAN JINGHE CHEM
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