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Application of an adsorption process in the synthesis of o-cresol novolac epoxy resin

A technology of novolac epoxy resin and phenolic resin, which is applied in the field of organic polymer compound synthesis, can solve the problems of long two-phase separation time, unstable separation time, and poor elution effect, so as to reduce emulsification and shorten washing time , Improve the effect of washing efficiency

Active Publication Date: 2022-07-22
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of washing with water after filtration in the closed-loop reaction of this method, there are technical deficiencies such as long two-phase separation time, unstable separation time, poor elution effect, and emulsification during the washing process using a centrifugal extractor, which cannot be separated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] This embodiment includes the following steps:

[0021] Step 1, dissolve 100g o-cresol resin in 50g methyl isobutyl ketone in the reaction kettle to obtain o-cresol resin solution, then add 150g epichlorohydrin and 5g reducing agent zinc powder to the o-cresol resin solution , and heated to 80°C for reduction and decolorization of o-cresol resin for 0.5h;

[0022] Step 2, add 5g phase transfer agent benzyl triethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide to the reaction system after the reduction and decolorization reaction in step 1 under vacuum conditions, at a pressure of 900mbar, temperature Under the condition of 80°C, the etherification reaction was carried out under reduced pressure and reflux for 3 hours to obtain the etherification reaction product;

[0023] Step 3, adding 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in step 2 under vacuum conditions, and carrying out a closed-loop rea...

Embodiment 2

[0027] This embodiment includes the following steps:

[0028] Step 1, dissolve 100g o-cresol resin in 50g methyl isobutyl ketone in the reaction kettle to obtain o-cresol resin solution, then add 150g epichlorohydrin and 5g reducing agent zinc powder to the o-cresol resin solution , and heated to 80°C for reduction and decolorization of o-cresol resin for 0.5h;

[0029] Step 2, add 5g phase transfer agent benzyl triethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide to the reaction system after the reduction and decolorization reaction in step 1 under vacuum conditions, at a pressure of 900mbar, temperature Under the condition of 80°C, the etherification reaction was carried out under reduced pressure and reflux for 3 hours to obtain the etherification reaction product;

[0030] Step 3, adding 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in step 2 under vacuum conditions, and carrying out a closed-loop rea...

Embodiment 3

[0034] This embodiment includes the following steps:

[0035] Step 1, dissolve 100g o-cresol resin in 50g methyl isobutyl ketone in the reaction kettle to obtain o-cresol resin solution, then add 150g epichlorohydrin and 5g reducing agent zinc powder to the o-cresol resin solution , and heated to 80°C for reduction and decolorization of o-cresol resin for 0.5h;

[0036] Step 2, add 5g phase transfer agent benzyl triethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide to the reaction system after the reduction and decolorization reaction in step 1 under vacuum conditions, at a pressure of 900mbar, temperature Under the condition of 80°C, the etherification reaction was carried out under reduced pressure and reflux for 3 hours to obtain the etherification reaction product;

[0037]Step 3, adding 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in step 2 under vacuum conditions, and carrying out a closed-loop reac...

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Abstract

The invention discloses an application of an adsorption process in the synthesis of o-cresol novolac epoxy resin, comprising: 1. dissolving the o-cresol novolac resin in an organic solvent, adding epichlorohydrin and a reducing agent, and heating for reduction and decolorization reaction; 2. Add a phase transfer agent and a cocatalyst to the reaction system after the reduction and decolorization reaction, carry out the etherification reaction under reduced pressure and reflux to obtain the etherification reaction product; The reaction system after the closed-loop reaction is filtered to obtain a feed liquid, which is then adsorbed by an adsorbent, washed with water, and distilled under reduced pressure to obtain o-cresol novolac epoxy resin. The invention adopts the adsorbent to adsorb the feed liquid of the reaction system after the closed-loop reaction, reduces the impurity content in the liquid after adsorption, improves the subsequent washing efficiency, shortens the washing time, reduces the emulsification phenomenon, and reduces the o-cresol aldehyde ring. Oxygen resin color and ensure low chlorine content of o-cresol epoxy resin.

Description

technical field [0001] The invention belongs to the technical field of organic polymer compound synthesis, in particular to the application of an adsorption process in the synthesis of o-cresol novolac epoxy resin. Background technique [0002] o-Cresol epoxy resin is a multifunctional glycidyl ether type epoxy resin. When the softening point of the resin changes, the epoxy value basically does not change, and the melt viscosity is quite low, which gives the molding compound resin excellent process stability. Machinability, and widely used in the semiconductor industry as the main bonding material for packaging materials such as LSI, VLSI integrated circuits, electrical components and civilian weak current products (VTR, OP). Electrical components encapsulated with high-purity resin can maintain good electrical insulation performance even in high temperature and humid environments. O-cresol epoxy resin, which is the main raw material of epoxy molding compound, besides softe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/02C08G59/14
CPCC08G59/025C08G59/145
Inventor 张玮辛昭陈黎马少波王罡
Owner XIAN ORIGIN CHEM TECH
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