A kind of 4-tert-alkylphenol-(phenol-based) formaldehyde resin and its preparation method and application

A technology of tertiary alkylphenol and phenolic resin, which is applied in the field of phenolic resin, can solve problems such as decreased adhesion, poor production safety, high temperature and high pressure required for production, etc., achieves improved initial viscosity and sticky durability, high safety, and improved production efficiency effect

Active Publication Date: 2021-11-23
SHANDONG YANGGU HUATAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adding p-tert-butylphenol formaldehyde resin and p-tert-octylphenol formaldehyde resin to the rubber compound has higher initial viscosity, but the adhesion drops sharply under storage, aeration or humid heat environment; p-tert-butylphenol acetylene resin production Requires high temperature and high pressure, poor production safety

Method used

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  • A kind of 4-tert-alkylphenol-(phenol-based) formaldehyde resin and its preparation method and application
  • A kind of 4-tert-alkylphenol-(phenol-based) formaldehyde resin and its preparation method and application
  • A kind of 4-tert-alkylphenol-(phenol-based) formaldehyde resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh 158.13g of 95 wt% p-tert-butylphenol, 103.8g of 99.7 wt% p-hydroxybenzaldehyde and 300g of toluene into the reaction kettle, raise the temperature to dissolve the raw materials, add 4.7g of oxalic acid and stir evenly. Reflux condensation reaction for 2.5 hours, add liquid caustic soda to neutralize to neutrality, then raise the temperature to distill out toluene and water, basically anhydrous and then raise the temperature to 160-180°C for polycondensation reaction, the polycondensation reaction time is 2.5 hours, after the reaction Pour out the product in the reaction kettle, and cool to obtain the 4-tert-alkylphenol-(phenol-based) formaldehyde resin of the present invention. The softening point detected by the ring and ball softening point instrument is 142 ° C, and the free phenol detected by the high performance liquid chromatography is 0.08 %, the weight average molecular weight detected by gel chromatography is 1240.

Embodiment 2

[0048] Weigh 158.13g of 95 wt% p-tert-butylphenol, 97.7g of 99.7 wt% p-hydroxybenzaldehyde and 270g of toluene into the reaction kettle, heat up to dissolve the raw materials, add 3.2g of concentrated sulfuric acid and stir evenly, at 98~102℃ Under reflux condensation reaction for 2.0 hours, add liquid caustic soda to neutralize to neutrality, then raise the temperature to distill toluene and water out, basically anhydrous and then raise the temperature to 150-170°C for polycondensation reaction, the polycondensation reaction time is 2.0 hours, the reaction After that, the product in the reaction kettle is poured out, cooled to obtain the 4-tert-alkylphenol-(phenol-based) formaldehyde resin of the present invention, and the softening point is 134°C as detected by a ring and ball softening point instrument, and the free phenol is detected by a high-performance liquid chromatography. It was 0.13%, and the weight average molecular weight detected by gel chromatography was 970.

Embodiment 3

[0050] Weigh 158.13g of 95 wt% p-tert-butylphenol, 109.91g of 99.7 wt% p-hydroxybenzaldehyde and 350g of toluene into the reaction kettle, heat up to dissolve the raw materials, add 3.5g of p-toluenesulfonic acid and stir evenly, at 100~ Reflux condensation reaction at 105°C for 3.5 hours, then raise the temperature to distill out toluene and water, then heat up to 160-180°C for polycondensation reaction, the reaction time is 3.5 hours, after the reaction is completed, the product in the reactor is Pour out and cool to obtain 4-tert-alkylphenol-(phenol-based) formaldehyde resin of the present invention. The softening point detected by the ring and ball softening point instrument is 141° C., and the free phenol detected by high performance liquid chromatography is 0.10%. Instrument detection weight average molecular weight is 1580.

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Abstract

The invention discloses a 4-tert-alkylphenol-(phenol-based) formaldehyde resin and its preparation method and application. It is prepared from p-hydroxybenzaldehyde and 4-tert-alkylphenol through condensation and polycondensation reactions. The method of the invention has simple operation, easy implementation, mild conditions, no high pressure, high safety, strong controllability, high product yield, good quality, energy saving and environmental protection. The methyl groups of the obtained resin are connected with phenol groups, which increases the content of phenolic hydroxyl groups per unit mass of the tackifying resin. The resin is especially suitable for use as a long-term tackifying resin for rubber in the manufacture and production of tires. The initial viscosity and viscous lasting power of the sizing material added with the resin of the present invention are greatly improved, can reduce the defective rate of tires or rubber products, can improve the quality of tires or rubber products, reduce production costs and increase production efficiency, and have great advantages. Good economic and social benefits.

Description

technical field [0001] The invention relates to a phenolic resin containing phenol groups, in particular to a 4-tert-alkylphenol-(phenol-based) formaldehyde resin, and also relates to its preparation method and its application as a tackifying resin for rubber, belonging to the technical field of phenolic resins . Background technique [0002] In the processing of rubber tires or products, especially in the processing of radial tires and bias tires, the bonding method is often used for molding, which requires the unvulcanized rubber to have a high molding viscosity. Natural rubber has good self-adhesiveness, so the process performance is good, while synthetic rubber has wear resistance, aging resistance and other advantages, but its self-adhesiveness is poor, which brings difficulties to the molding process, thus limiting the use of synthetic rubber. [0003] If there is no viscosity between the rubber materials, especially for synthetic rubber compounds, the semi-finished r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G8/04C08L9/06C08L61/06C08K13/02C08K3/22C08K5/09C08K3/06C08K3/04
Inventor 李剑波王文博杜孟成李庆朝郭庆飞
Owner SHANDONG YANGGU HUATAI CHEM
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