Method for synthesizing light color low-chlorinity o-cresol-formaldehyde epoxy resin

A novolac epoxy resin and synthesis method technology, applied in the field of organic polymer compound synthesis, can solve the problems of high loss of epichlorohydrin, not strict equipment requirements, poor color of products, etc., and achieve the effect of reducing side reactions and reducing losses

Active Publication Date: 2013-01-30
THE NORTHWEST RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The one-step process has strict requirements on equipment, and the process control automation degree is high, and the investment is large; the two-step process has no strict requirements on equipment, and the control is simple, but the product color is poor; the other two processes use one of the raw materials. Oxychlorohydrin is used as a medium solvent for etherification and ring-closing reactions, resulting in a large loss of epichlorohydrin

Method used

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  • Method for synthesizing light color low-chlorinity o-cresol-formaldehyde epoxy resin

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Step 1, add o-cresol aldehyde resin 100g, organic solvent methyl isobutyl ketone 500g in reaction kettle, obtain o-cresol aldehyde resin solution, then add epichlorohydrin 150g and reducing agent zinc powder 5g in o-cresol aldehyde resin solution , heating up to 80°C for reduction decolorization reaction for 0.5h;

[0026] Step 2. Under vacuum conditions, add 5 g of phase transfer catalyst benzyltriethylammonium chloride (TEBA) and 3 g of cocatalyst sodium hydroxide to the reaction system after the reduction decolorization reaction in step 1, and the pressure is 900 mbar. Etherification reaction at 80°C for 3 hours to obtain etherification reaction product;

[0027] Step 3. Under vacuum conditions, add 45 g of NaOH solution with an alkali catalyst mass concentration of 55% to the etherification reaction product described in step 2, and perform a ring-closure reaction at a pressure of 900 mbar and a temperature of 90° C. for 8 h;

[0028] Step 4, filter the reaction sys...

Embodiment 2

[0030] The present embodiment is the same as Example 1, except that the organic solvent is 250 g each of methyl isobutyl ketone and cyclohexanone; the reducing agent is 3 g of Zn powder and 2 g of Al powder; the phase transfer catalyst Be tetrabutylammonium bromide 2g, benzyltriethylammonium chloride 3g; Described promotor is sodium hydroxide and potassium hydroxide total 3g, wherein sodium hydroxide and potassium hydroxide mass ratio 1: 1; Described The alkali catalyst is 45 g of a mixture solution of 55% sodium hydroxide and potassium hydroxide, wherein the mass ratio of sodium hydroxide to potassium hydroxide is 1:1.

Embodiment 3

[0032] Step 1, add o-cresol novolac resin 100g, organic solvent toluene 700g in reaction kettle, obtain o-cresol novolac resin solution, then add epichlorohydrin 200g and reducing agent zinc powder 2g in o-cresol novolac resin solution, be warming up to 50 ℃ reduction decolorization reaction 1h;

[0033] Step 2. Under vacuum conditions, add 0.5 g of phase transfer catalyst tetrabutylammonium bromide and 1 g of cocatalyst potassium hydroxide to the reaction system after the reduction decolorization reaction in step 1. The pressure is 900 mbar and the temperature is 80 ° C. Under the etherification reaction for 7h, the etherification reaction product was obtained;

[0034] Step 3. Under vacuum conditions, add 60 g of ammonium hydroxide solution with an alkali catalyst mass concentration of 50% to the etherification reaction product described in step 2, and perform a ring-closure reaction at a pressure of 400 mbar and a temperature of 80° C. for 10 h;

[0035]Step 4, filter the ...

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Abstract

The invention discloses a method for synthesizing a light color low-chlorinity o-cresol-formaldehyde epoxy resin. The method comprises the following steps of: 1, dissolving o-cresol-formaldehyde resin in an organic solvent to obtain an o-cresol-formaldehyde resin solution, adding epoxy chloropropane and a reductant into the o-cresol-formaldehyde resin solution for reductive decoloration reaction of the o-cresol-formaldehyde resin; 2, adding a phase transfer catalyst and a cocatalyst into the reaction system and refluxing under reduced pressure and performing etherification reaction; 3, adding an alkali catalyst into a product of etherification reaction and performing ring-closure reaction; and 4, filtering, washing, reducing pressure and removing the solvent and the unreacted epoxy chloropropane from washed entrapment materials to obtain the light color low-chlorinity o-cresol-formaldehyde epoxy resin of which the Gardner chromaticity is not more than 1 and the chlorinity is not more than 200 ppm. The o-cresol-formaldehyde epoxy resin prepared by the method can meet the requirements for softening point and epoxy value, and is characterized in that the chlorine ion content in the o-cresol-formaldehyde epoxy resin is very low and is less than 200 ppm, and the Gardner chromaticity of the o-cresol-formaldehyde epoxy resin is not more than 1.

Description

technical field [0001] The invention belongs to the technical field of synthesis of organic polymer compounds, and in particular relates to a method for synthesizing light-colored o-cresol-formaldehyde epoxy resin with low chlorine content. 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. And processing technology, so it is widely used in the semiconductor industry as the main bonding material for packaging materials such as LSI, VLSI integrated circuits, electronic components and civilian weak products (VTR, OP). Electronic components encapsulated with high-purity resin can maintain their good electrical insulation properties even in high temperature and humid environments. As the main raw material of epoxy moldin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/08
Inventor 辛昭张玮赵杨锋韩肖慧
Owner THE NORTHWEST RES INST OF CHEM IND
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