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Method for preparing phenolic resin by adopting pyrrole acidic ionic liquid as catalyst

A technology of acidic ionic liquid and phenolic resin, which is applied in the field of ionic liquid catalysis, can solve the problems of low catalyst activity, long time consumption, and low yield, and achieve the effects of good selectivity, high yield, and simple preparation

Inactive Publication Date: 2019-04-05
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of low catalyst activity, long time-consuming preparation process of phenolic resin microspheres, and low yield of target pellets with a diameter of 0.8 to 1.0 mm in the prior art, and to provide a method for preparing phenolic resin by using acidic ionic liquid catalysis Resin pellet method

Method used

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  • Method for preparing phenolic resin by adopting pyrrole acidic ionic liquid as catalyst
  • Method for preparing phenolic resin by adopting pyrrole acidic ionic liquid as catalyst
  • Method for preparing phenolic resin by adopting pyrrole acidic ionic liquid as catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Add the N-methylpyrrolidone of 0.1mol in the 250ml four-neck flask with mechanical stirring device, slowly add the 98% sulfuric acid of the amount of equal substance with constant pressure funnel under ice bath, control rate at 10s / drop, in case The reaction was too violent; after the dropwise addition was completed, it was stirred in a water bath at 60°C for 24h. The obtained liquid was repeatedly washed three times with ethyl acetate, and after rotary evaporation and vacuum drying, a light yellow viscous ionic liquid (1) N-methylpyrrolidone bisulfate ([Hnmp]HSO 4 ).

[0022] Add phenol (P) and formaldehyde (F) with a molar ratio of 1:0.75 in a 1000ml three-neck flask equipped with a condensing reflux tube and a stirrer, use pyrrole acidic ionic liquid as a catalyst, and add 0.2wt% ionic liquid (1) Heat to reflux state while stirring, keep this state for 2 hours, then add 8wt% polyvinyl alcohol (PVA) aqueous solution, keep reflux state and continue to stir and disper...

Embodiment 2

[0024] Add 0.1mol of N-methylpyrrolidone in a 250ml four-necked flask with a mechanical stirring device, and slowly add 80% phosphoric acid with a constant pressure funnel under an ice bath to control the rate at 10s / drop to prevent The reaction was too violent; after the dropwise addition was completed, it was stirred in a water bath at 60°C for 24h. The obtained liquid was repeatedly washed three times with ethyl acetate, and after rotary evaporation and vacuum drying, a light yellow viscous ionic liquid (2) N-methylpyrrolidone bisulfate ([Hnmp]HSO 4 ).

[0025] In the 1000ml there-necked flask that condensing reflux tube, stirrer are equipped with, add the resorcinol (P), formaldehyde (F) that mol ratio is 1:0.9, take pyrrole acidic ionic liquid as catalyst, add 0.3wt% ionic liquid ( 2) heating to reflux state while stirring, keep this state for 0.5h, then add 8wt% polyvinyl alcohol (PVA) aqueous solution, keep reflux state and continue to stir and disperse for 40min, fina...

Embodiment 3

[0028] Add 0.1mol of N-methylpyrrolidone in a 250ml four-necked flask with a mechanical stirring device, and slowly add the p-toluenesulfonic acid aqueous solution of the amount of the same substance with a constant pressure funnel under ice bath, and control the rate at 10s / drop, In case the reaction is too violent; after the dropwise addition, stir in a water bath at 60°C for 24h. The obtained liquid was repeatedly washed three times with ethyl acetate, and after rotary evaporation and vacuum drying, a light yellow viscous ionic liquid (3) N-methylpyrrolidone bisulfate ([Hnmp]HSO 4 ).

[0029] Add p-cresol (P) and formaldehyde (F) with a molar ratio of 1:0.8 in a 1000ml three-necked flask equipped with a condensing reflux tube and a stirrer, use pyrrole acidic ionic liquid as a catalyst, and add 0.5wt% ionic liquid (3) Heat to reflux state while stirring, keep this state for 1.0h, then add 8wt% polyvinyl alcohol (PVA) aqueous solution, keep reflux state and continue stirrin...

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Abstract

The invention belongs to the field of ionic liquid catalysis, in particular to a method for preparing phenolic resin by adopting a pyrrole acidic ionic liquid as a catalyst. The method includes adopting phenol and formaldehyde as raw materials and the pyrrole acidic ionic liquid as a catalyst to catalyze and prepare the phenolic resin; and after the reaction is finished, filtering and separating phenolic resin balls when the resin is hot, cooling the filtrate water phase to below 10 DEG C, automatically separating the ionic liquid and the water, and separating the pyrrole acidic ionic liquid to reuse. The ionic liquid adopted by the method has the advantages of simple preparation process, low price, high catalyst efficiency, short condensation reaction time, reusability of the ionic liquid, smooth surface of the prepared phenolic resin balls, uniform diameter of the balls, and high yield of products with a target bead diameter of 0.8-1.0 mm.

Description

technical field [0001] The invention belongs to the field of ionic liquid catalysis, and in particular relates to a method for preparing phenolic resin by using pyrrole acidic ionic liquid as a catalyst. Background technique [0002] As one of the three major thermosetting resins, phenolic resin has gained industrial recognition due to its easy-to-obtain raw materials, low price, simple and mature production process, low investment in manufacturing and processing equipment, easy molding, and performance after curing to meet various requirements. Wide range of applications. At present, the process of synthesizing phenolic resin balls adopts traditional techniques (Qin Zhengyong. Preparation and application of phenolic resin-based spherical activated carbon [D]. East China University of Science and Technology, 2012.), using inorganic acids and bases as catalysts, the synthesis process is complicated and time-consuming Longer, the condensation reaction lasts for more than ten ...

Claims

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Application Information

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IPC IPC(8): C08G8/10
CPCC08G8/10
Inventor 李为民李娜张杨任庆功
Owner CHANGZHOU UNIV
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