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Method for manufacturing phenol resin using ion exchange resin as catalyst

A technology of ion exchange resin and phenol resin, applied in the field of resin, can solve the problems of phenol water pollution, complicated auxiliary process, equipment corrosion, etc.

Inactive Publication Date: 2004-01-28
夏红元
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the production process, in addition to the serious corrosion of the equipment, these catalysts must also be neutralized, washed with water and other complex auxiliary processes, and the serious problem of environmental pollution by phenolic water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0010] Example 1. Preparation of Resin Catalyst

[0011] Ion-exchange the macroporous D72 ion-exchange resin with 5% aqueous hydrochloric acid solution 4 times the volume of the resin into a hydrogen-form resin. water, pour the wet resin into a tray, dry it in an oven at 120°C, and store it for later use.

[0012] The preparation of p-tert-butylphenol formaldehyde resin:

[0013] Get 25g of p-tert-butylphenol, 17ml of 35% formaldehyde, 100ml of toluene solution, and 25g of the hydrogen-type D72 resin catalyst prepared above, and add them successively to a 250ml four-necked flask with a reflux condenser and a stirrer, slowly heat up, and stir simultaneously , react at the reflux temperature for 2 hours, note that when using the new resin catalyst for the first time, there will be an exothermic peak at about 80°C before the reflux temperature, and attention should be paid to control, and then the reaction liquid and the catalyst are separated, and the separated catalyst Can be...

example 2

[0015] The D72 resin catalyst 100g after the hydrogen type drying of example 1 method system, p-tert-butyl phenol 300g, 37% formaldehyde 180cm^3 is added in 1000cm^3 band reflux, the four-necked bottle of stirring, to the first use The resin catalyst must pay attention to temperature control and slowly heat, and react at reflux temperature for 2 hours. Then the reaction solution is separated from the catalyst. Note that because the solvent-free system is relatively viscous, it needs to be separated rapidly at a higher temperature. The catalyst can be reused, and the reused catalyst has no exothermic peak. The reaction liquid was heated in a 1000cm^3 flask, vacuumed and dehydrated. When the liquid phase temperature reached 150°C, the operation was stopped, and the product was poured out while it was hot to obtain about 330g of resin with a softening point of about 100°C.

example 3

[0017] Add 25g of the hydrogen-type dried D72 resin catalyst, 100g of phenol, and 80ml of 37% formaldehyde prepared by the method of Example 1 into a 500ml four-necked flask with reflux and stirring, and pay attention to temperature control for the resin catalyst used for the first time. Slowly heat, or add formaldehyde in batches, react at reflux temperature for 3 hours, then separate the reaction solution from the catalyst, and the catalyst can be reused. The reactant was heated in a 500ml flask, and vacuum dehydrated at 0.07Mpa. When the liquid phase temperature reached 150°C, the operation was stopped, and the product was poured out while it was hot to obtain about 110g of phenolic resin with a softening point of about 100°C.

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Abstract

The present invention discloses a method for synthesizing phenol resin ion exchange resin as catalyst. Said method includes: using 5% hydrochloric acid to treat macroporous cation exchange resin, when the exchange equivalent determined is 3.0-5.0 mg equivalent / g, using lots of distilled water to wash exchanged resin to neutrality, filtering and removing free water, pouring the resin into disk, drying at 90-120 deg.C in drying over for stand-by; mixing phenols of phenol, bisphenol A and p-tert-butylphenol, etc. and aldehydes of formaldehyde and acetaldehyde, etc. according to the mole ratio of1:0.5-1:2, and under the catalysis of the hydrogen-type macroporous cation exchange resin according to weight percentage of 15-50%, in the presence of solvent toluene or xylene or in non-solvent system.

Description

technical field [0001] The present invention relates to resins, and more specifically, the present invention relates to a method for preparing phenolic resins using ion exchange resins as catalysts. Background technique [0002] At present, phenolic resin is still the main synthetic resin, and most of the catalysts used in the production process of linear phenolic resin are sulfuric acid, hydrochloric acid, benzenesulfonic acid, oxalic acid, etc. In the production process, these catalysts not only cause serious corrosion to the equipment, but also a series of auxiliary processes such as neutralization and water washing are complicated, and there is a serious problem of phenolic water polluting the environment. Contents of the invention [0003] The purpose of the present invention is to use strongly acidic cation exchange resin as a catalyst for the polycondensation reaction of phenol and aldehyde, overcome the shortcom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G8/10
CPCY02P20/582
Inventor 夏红元
Owner 夏红元
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