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Application of adsorption process in synthesis of o-cresol formaldehyde epoxy resin

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

Active Publication Date: 2020-04-21
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, 100g o-cresol novolac resin is dissolved in 50g methyl isobutyl ketone in reactor, obtain o-cresol novolac resin solution, then add 150g epichlorohydrin and 5g reducing agent zinc powder in o-cresol novolac resin solution , and heated to 80°C for reduction and decolorization of o-cresol novolac resin for 0.5h;

[0022] Step 2, add 5g phase transfer agent benzyltriethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide in the reaction system after reduction decolorization reaction in step 1 under vacuum condition, be 900mbar at pressure, 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. Add 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in Step 2 under vacuum conditions, and perform a ring closure reac...

Embodiment 2

[0027] This embodiment includes the following steps:

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

[0029] Step 2, add 5g phase transfer agent benzyltriethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide in the reaction system after reduction decolorization reaction in step 1 under vacuum condition, be 900mbar at pressure, 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. Add 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in Step 2 under vacuum conditions, and perform a ring closure reac...

Embodiment 3

[0034] This embodiment includes the following steps:

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

[0036] Step 2, add 5g phase transfer agent benzyltriethylammonium chloride (TEBA) and 3g cocatalyst sodium hydroxide in the reaction system after reduction decolorization reaction in step 1 under vacuum condition, be 900mbar at pressure, 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. Add 45 g of NaOH solution with a mass concentration of 55% to the etherification reaction product obtained in Step 2 under vacuum conditions, and perform a ring closure react...

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Abstract

The invention discloses application of an adsorption process in o-cresol formaldehyde epoxy resin synthesis. The process comprises the following steps: 1, dissolving o-cresol formaldehyde resin in anorganic solvent, adding epoxy chloropropane and a reducing agent, and carrying out heating to perform a reductive decolorization reaction; 2, adding a phase transfer agent and a cocatalyst into the reaction system having undergone the reductive decolorization reaction, and carrying out reduced-pressure reflux for an etherification reaction to obtain an etherification reaction product; 3, adding abase catalyst into the etherification reaction product for a ring-closure reaction; and 4, filtering the reaction system having undergone the ring-closure reaction to obtain a feed liquid, subjectingthe feed liquid to adsorption with an adsorbent, carrying out washing with water, and carrying out reduced-pressure distillation to obtain the o-cresol formaldehyde epoxy resin. According to the method, the adsorbent is used for adsorbing the reaction system feed liquid after the ring-closure reaction, so the content of impurities in the liquid after adsorption is reduced, subsequent washing efficiency is improved, washing time is shortened, the phenomenon of emulsification is reduced, the chromaticity of the o-cresol formaldehyde epoxy resin is reduced, and the low chlorine content of the o-cresol formaldehyde epoxy resin is ensured.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organic polymer compounds, and in particular relates to the application of an adsorption process in the synthesis of o-cresol novolak epoxy resin. Background technique [0002] O-cresol novolac epoxy resin is a polyfunctional 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 endows the molding compound resin with excellent process stability. Machining technology, 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. As the main raw material of epoxy molding compound, o-cre...

Claims

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Application Information

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Patent Type & Authority Applications(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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