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Solvent-free method for preparing tackified p-tert-butyl phenolic resin

A technology of p-tert-butylphenol and p-tert-butyl, which is applied in the field of solvent-free preparation of tackified p-tert-butylphenol resin, can solve problems such as environmental pollution and inevitable solvent volatilization damage, and achieve reduced production costs and improved product performance. Improve and avoid the effect of violent gathering

Active Publication Date: 2010-06-09
WUHAN JINGHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Generally, inert solvents such as toluene and methanol are added after the phenolic reaction is completed, water is added to separate the layers, the water phase is discharged, and then the solvent is recovered by heating, which will inevitably cause the volatilization of the solvent and the harm to the human body, and also cause environmental pollution.

Method used

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  • Solvent-free method for preparing tackified p-tert-butyl phenolic resin
  • Solvent-free method for preparing tackified p-tert-butyl phenolic resin
  • Solvent-free method for preparing tackified p-tert-butyl phenolic resin

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Add 150g of p-tert-butylphenol and 25g of formaldehyde into a 500mL three-necked flask, slowly heat up and melt, and stop the temperature rise when it reaches 90-95°C. Stir for 15 to 30 minutes, add 8.45 g of catalyst (hydrochloric acid) dropwise under reflux, finish adding in about 1.5 hours, and reflux at 101°C for 3 hours. After the reaction, 0.55 g of sodium dodecylbenzenesulfonate was added and stirred for 10 to 20 minutes. Heating and dehydration, when the system is 110°C, it becomes transparent, continue to heat up to 170-180°C, add 1.2g of oxalic acid, stir for 10-20 minutes, vacuum dehydration for 20 minutes (vacuum degree > 0.085MPa); stop the reaction, pour out the material, After cooling, a light yellow transparent flaky solid was obtained.

Embodiment 2

[0043] Add 400g of p-tert-butylphenol and 41.6g of formaldehyde into a 1L three-neck flask, slowly heat up and melt, and stop the temperature rise when it reaches 90-95°C. After stirring for 20 minutes, 22.5 g of the catalyst (hydrochloric acid) was added dropwise under reflux, and the addition was completed in about 1.5 hours, followed by reflux at 101° C. for 3 hours. After completion of the reaction, 0.92 g of sodium dodecylbenzenesulfonate was added, followed by stirring for 10 to 20 minutes. Heat up and dehydrate, when the system is 110°C, it becomes transparent, continue to heat up to 170-180°C, add 2g of oxalic acid, stir for 10-20 minutes, vacuum dehydrate for 20 minutes (vacuum degree > 0.085MPa); stop the reaction, pour out the material, cool A light yellow transparent flaky solid was obtained.

Embodiment 3

[0045] Add 55kg of p-tert-butylphenol and 19kg of formaldehyde into a 200L reactor, slowly heat up and melt until it reaches 90-95°C, then stop the temperature rise. Stir for 15-30 minutes, add 6.5 kg of catalyst (hydrochloric acid) dropwise under reflux, finish adding in about 1.5 hours, and reflux at 101°C for 3 hours. After the reaction was completed, 0.4 kg of sodium dodecylbenzenesulfonate was added and stirred for 10 to 20 minutes. Heat up and dehydrate, when the system is 110°C, it becomes transparent, continue to heat up to 170-180°C, add 0.9kg oxalic acid, stir for 10-20 minutes, vacuum dehydrate for 25 minutes (vacuum degree > 0.085MPa); stop the reaction, pour out the material, After cooling, a light yellow transparent flaky solid was obtained.

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Abstract

A solvent-free method for preparing trackifying para-tertiary butyl phenol phenolic resin comprises the following components and dosage, with the dosage of weight part: 900-1000 parts of para-tertiarybutyl phenol, 150-200 parts of 97% formaldehyde, 40-50 parts of 10% hydrochloric acid, 5-10 parts of oxalic acid, and 1.5-3.5 parts of surface-active agent, wherein, 97% formaldehyde and 10% hydrochloric acid are both weight percentage. The method overcomes the shortcoming of the existing method for preparing para-tertiary butyl phenol phenolic resin, which uses solvent; and the method has the advantages of simple synthetic process, low production cost and higher performance than that of the existing product, and avoids sudden gathering in the process of preparation, and the like.

Description

technical field [0001] The invention relates to a new method for improving the process of tackifying phenolic resin for rubber, more specifically, it is a method for preparing tackifying p-tert-butylphenolic resin without solvent. technical background [0002] Adhesion is an extremely complex phenomenon. So far, the mechanism of action of alkylphenol-formaldehyde resins in adhesion is not very clear, but most researchers believe that: first, because the substituents on the phenolic ring have a certain degree of branching, good flexibility, and rubber molecules It has good compatibility. When hot mixing, the resin and rubber interact as if they are in a solvent, which is similar to colloidal mixing, which increases the free movement of rubber molecules. Second, the phenolic hydroxyl groups in the resin have a certain polarity, and the hydrogen on the hydroxyl groups has the ability to form hydrogen bonds. During the mixing process, they form an interpenetrating hydrogen bond...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/12
Inventor 王腊生严建国熊斌袁春香刘建斌卢建设方绍敏童凡刘金恬
Owner WUHAN JINGHE CHEM
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