Method for preparation of phenolic resin by two-phase technique

A technology of phenolic resin and phenol, applied in the field of preparation of phenolic resin, can solve the problems of easily causing volatility, unfavorable rubber, loss of catalytic ability, etc., and achieves the effect of reducing moisture and improving efficiency

Active Publication Date: 2014-07-16
SINO LEGEND CHINA CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In other preparations of low-distribution phenolic resin processes, generally weak acids are used as catalysts to make the reaction process mild and easy to control, such as the use of malic acid, tartaric acid, etc. disclosed in CN1183421A; the organic phosphoric acid used in CN 1303877A; but , in the process of catalytic reaction, the catalytic efficiency of weak acid is low, and the temperature must be controlled accurately. For example, the decomposition temperature of malic acid is 140°C, and the dehydration temperature of phenol-formaldehyde resin is generally 130-160°C, which is easy to make Malic acid decomposes and loses its catalytic ability; although organophosphoric acid is relatively stable, it is difficult to remove in the system, and in the subsequent use process, especially as a reinforcing resin for rubber tires, it is easy to cause volatilization, which is very difficult for the use of rubber It is unfavorable, so organophosphoric acid cannot be used as a catalyst for the preparation of reinforced resin for rubber

Method used

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  • Method for preparation of phenolic resin by two-phase technique
  • Method for preparation of phenolic resin by two-phase technique
  • Method for preparation of phenolic resin by two-phase technique

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preparation example Construction

[0024] The preparation method of the present invention specifically comprises: in a four-necked flask equipped with a stirring device, an electric heating temperature control device and a reflux condenser, add about 100-200 g of toluene solvent, then add 100-200 g of phenol, and 37% of Formaldehyde 50~100g, heat up to 100°C. And add 0.5-5g of benzenesulfonic acid catalyst, reflux reaction for 1-3h, after the reaction, raise the temperature to 130-150°C, carry out atmospheric distillation for 1h, remove excess water and solvent, add organic amines The terminator is used to terminate the reaction. In this experiment, 1,8-diazabicyclo[5.4.0]undec-7-ene (abbreviated as DBU) was used to terminate the reaction. Its structural formula is as follows to obtain the product phenolic resin.

[0025]

Embodiment 1

[0027] Add 100g of toluene, 150g of phenol and 1.8g of benzenesulfonic acid into a 500ml four-neck flask, raise the temperature to 100°C and start stirring slowly, then slowly add 20g of 37% liquid aldehyde to the system dropwise for 30min; Then slowly add 13.5g of solid aldehyde, and finish adding in 30 minutes; finally add 26.7g of liquid aldehyde dropwise, and finish adding dropwise within 30 minutes. The system is milky white. Reflux reaction at 100°C for 1 hour, then increase the temperature to 130°C, remove water and toluene respectively, the solution gradually changes from milky white to light red or dark red, until no substance comes out from the distillation reaction, add 0.64g DBU, there will be a lot of white Fog is formed, stir for 5-10 minutes, stop stirring and discharge to obtain a reddish-brown solid.

Embodiment 2

[0031] Add 100g of toluene, 150g of phenol and 1.8g of benzenesulfonic acid into a 500ml four-neck flask, raise the temperature to 100°C and start stirring slowly, then slowly add 20g of 37% liquid aldehyde to the system dropwise for 30min; Then slowly add 13.5g of solid aldehyde, 30min after the addition is complete, after the reflux reaction, a large amount of foam will be generated, which is caused by the water reflux reaction in the system, and the system becomes milky white. Finally, 26.7 g of liquid aldehyde was added dropwise, and the same dropwise addition was completed within 30 minutes. Reflux at 100°C for 1 hour, then increase the temperature to 150°C, remove water and toluene respectively, the solution gradually changes from milky white to light red or dark red, until no substance comes out from the distillation reaction, add 0.64g DBU, there will be a lot of white Fog is formed, stir for 5-10 minutes, stop stirring and discharge to obtain a reddish-brown solid.

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Abstract

The invention discloses a method for preparation of phenolic resin by a two-phase technique. The method involves an organic solvent and a water solvent. Phenol and aldehyde are adopted as reactants, and a strong acid is taken as a catalyst. The reactants and the catalyst undergo reaction at the interface between the organic solvent and the water solvent to prepare the low molecular weight phenolic resin with narrow molecular weight distribution. The method provided by the invention uses the strong acid as the catalyst to shorten the reaction time, and the use of the strong acid as the catalyst has no adverse effect on subsequent use. The prepared phenolic resin is easy to disperse during application and can achieve even distribution.

Description

technical field [0001] The invention relates to a method for preparing a phenolic resin for rubber reinforcement, in particular to a method for preparing a phenolic resin with low molecular weight and narrow molecular weight distribution by using a two-phase method. Background technique [0002] Phenol formaldehyde resin is applied to the triangular filling rubber of the tire spigot. Before the rubber thinning, it can plasticize the rubber, improve the processing and mixing performance of the rubber; after thinning, it forms an interpenetrating network system with the rubber, Improve the hardness and tensile modulus of rubber, and improve the performance of rubber. For example, the application of phenolic resin as a rubber reinforcing material has been described in detail in "Combination of Rubber, Plastic and Synthetic Resin" (published in 1976, Petrochemical Press, Schwarz et al., Chapter 3). Most of the phenolic resins currently used in the market are modified phenol-for...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10C08G8/12C08G8/08C08L61/10C08L61/08
Inventor 张坤
Owner SINO LEGEND CHINA CHEM
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