Method for synthesizing o-cresol formaldehyde epoxy resin by using cosolvent and recovering cosolvent

A phenolic epoxy resin and phenolic resin technology, applied in the field of epoxy resin synthesis, can solve the problems of high production cost, large side reactions, difficult recovery of cosolvents, etc., and achieve the advantages of increasing yield, reducing hydrolysis and reducing the amount of waste polymer. Effect

Active Publication Date: 2015-05-20
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims at the problem of high production cost caused by large side reactions in the process of synthesizing o-cresol novolac epoxy resin by co-solvent method in the prior art, difficult recovery of co-solvent, and the purpose is to provide a method that can effectively reduce side reactions and recycling The preparation method of o-cresol novolac epoxy resin that utilizes co-solvent to reduce production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a four-neck flask with stirring, a thermometer, and a condenser, add 75g o-cresol novolac resin, 280g epichlorohydrin and 90g propylene glycol methyl ether. Under the protection of nitrogen, the temperature was raised to 60°C, and 4g of 50% NaOH was added for pre-reaction, and the pre-reaction was maintained for 4h. Reduce the vacuum to 13kPa and add 42g of 50% NaOH to carry out the cyclization reaction. At the same time, the reaction wastewater is separated by distillation, and the reaction time is 6h. Distillation reclaims epichlorohydrin and cosolvent to obtain crude resin, adds new epichlorohydrin 60g and reaction waste water to crude resin, after dissolving, let stand to separate liquids, distill and recover organic solvent, add 400g toluene to dissolve in remaining crude resin, Add 15g15%NaOH at a temperature of 80°C for 2h. After refining, add deionized water to wash until pH = 7-8, and remove the solvent.

[0024] The product indicators are as follows: yiel...

Embodiment 2

[0026] In Example 1, the pre-reaction, reaction and refined alkali were changed to 50% KOH, and all the other conditions were unchanged.

[0027] The obtained product indicators are as follows: epoxy resin yield: 104g, waste polymer amount: 0.87g, auxiliary agent recovery in wastewater: 14.2g, epoxy equivalent: 203.5g / eq, hydrolyzable chlorine 53ppm, inorganic chlorine 1ppm.

Embodiment 3

[0029] In a four-neck flask with stirring, thermometer and condenser, add 75g o-cresol novolac resin, 280g epichlorohydrin and 90g n-butanol. Under the protection of nitrogen, the temperature was raised to 65°C, and 4g of 50% NaOH was added for pre-reaction, and the pre-reaction was maintained for 4h. Reduce the vacuum to 13kPa and add 42g of 50% NaOH to carry out the cyclization reaction, and distill and separate the reaction wastewater at the same time, the reaction time is 6h; then distill and recover epichlorohydrin and co-solvent to obtain a crude resin, and add 60g of new epichlorohydrin to the crude resin and reaction waste water, after dissolving, let stand to separate the liquid, and distill to recover the organic solvent. Add 400g of methyl isobutyl ketone to the remaining crude resin to dissolve, add 15g of 15% NaOH at a temperature of 85°C and refine it for 2h. After refining, add deionized water to wash until pH = 7-8, and remove the solvent.

[0030] The produc...

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Abstract

The invention discloses a method for synthesizing o-cresol formaldehyde epoxy resin by using a cosolvent and recovering the cosolvent. The method comprises the following steps: mixing chloropropylene oxide with the cosolvent, adding the mixture into o-cresol formaldehyde resin, and carrying out a base catalysis pre-reaction; carrying out a base catalysis ring closure reaction, and carrying out reduced pressure distillation to separate out reaction wastewater; distilling the cosolvent and excess chloropropylene oxide after the ring closure reaction to obtain crude resin; and adding chloropropylene oxide and the wastewater obtained after the ring closure reaction into the crude resin, carrying out salt-out extraction, discharging the above obtained salt-out extracted water phase, distilling the above obtained organic phase to recover chloropropylene oxide and the cosolvent, and refining the remaining crude resin to obtain the o-cresol formaldehyde epoxy resin. The method has the advantages of effective enhancement of the ring closure reaction effect, reduction of the amount of polymer wastes, effective recovery and cycle use of the cosolvent, and great reduction of the production cost.

Description

technical field [0001] The invention relates to a method for synthesizing o-cresol novolac epoxy resin by using a cosolvent and recovering the cosolvent, belonging to the technical field of epoxy resin synthesis. Background technique [0002] O-cresol novolac epoxy resin has the characteristics of high heat resistance, low moisture absorption, and low thermal expansion coefficient, and is widely used in green electronic packaging, IC packaging, PCB ink and other fields. With the increase of the softening point of o-cresol novolak epoxy resin, the molecular chain of the resin gradually increases, the molecular chain is easy to curl, and the steric hindrance effect of the ortho-methyl group is also large, so the epoxy group is connected to the The difficulty increases in the phenolic molecular chain. This leads to a large number of side reactions in the reaction process, which are manifested in the increased consumption of epichlorohydrin and the increase of waste polymers in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/08C08J11/02
Inventor 肖雄任六波傅江福汤文红杨鑫
Owner CHINA PETROLEUM & CHEM CORP
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