Method for preparing epoxy resins of phenol formaldehyde type

A technology of epoxy resin and phenol formaldehyde, which is applied in the field of epoxidation, can solve the problems of insufficient etherification reaction, increase of resin chroma, and many side reactions of hydrolysis, so as to reduce hydrolysis side reactions, accelerate etherification reaction, reduce Occurrence Effects

Inactive Publication Date: 2008-12-31
ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, the process is immature, and it is difficult to synthesize a resin with a higher softening point. It is still in the experimental stage, and industrial production is difficult.
[0007] To sum up, the shortcomings of the traditional epoxidation reaction process are insufficient etherification reaction, many side reactions of hydrolysis, and the occurrence of heterotopic addition leads to more isomerized chlorine in the molecule, which makes subsequent refined dechlorination difficult and easy. The content of saponified chlorine is high, and the residual phenolic hydroxyl groups in the molecule are more oxidized into quinone structure, which increases the chroma of the resin and affects the storage stability. The high content of hydroxyl groups in the molecular structure results in a lot of emulsification loss by washing, resulting in low product yield and raw material consumption. advanced questions

Method used

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  • Method for preparing epoxy resins of phenol formaldehyde type

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Be that 105 ℃ of linear phenol formaldehyde resin 1000g with softening point and 6000g purity are 99.5% (weight) epichlorohydrin drop into reaction container, make system material be in purity (weight) be under the nitrogen protection of 99.5%, temperature control is at Dissolve at 80-82°C for 50 minutes to form a uniform transparent liquid, then control the reaction system at a vacuum of 0.082-0.083MPa, a temperature of 75±2°C, and an epichlorohydrin reflux rate of 1100-1200g / h, and add all at once 10g of benzyltriethylammonium chloride aqueous solution with a weight concentration of 50%, and keep it for 15 minutes, then add 820g of NaOH aqueous solution with a weight concentration of 48% to the system dropwise, and adjust and control the reflux rate at about 1100-1200g / h during the dropping process Carry out water separation and cyclization reaction, add sodium hydroxide solution evenly for 4 hours, maintain the etherification reaction for 2 hours under the same conditi...

Embodiment 2

[0036] Be that 1000g of matrix resin linear phenol-formaldehyde resin 1000g and 5000g purity are 99.5% (weight) epichlorohydrin drop into reaction container with softening point, make system material be in purity (weight) under the nitrogen protection of 99.5%, control Dissolve at 78-80°C for 40 minutes to form a uniform transparent liquid, then control the reaction system at a vacuum of 0.082-0.083MPa, a temperature of 75±2°C, and a reflux rate of epichlorohydrin of 1100-1200g / h. Add 8g of tetrabutylammonium chloride and tetramethylammonium chloride mixture aqueous solution with a weight concentration of 50% and keep it for 12 minutes, then add 800g of KOH aqueous solution with a weight concentration of 50% to the system dropwise, and keep the vacuum during the dropping process At 0.078-0.080MPa, the reaction temperature is 72-73°C, the reflux rate is controlled at about 1100-1200g / h to carry out the water separation cyclization reaction, and the potassium hydroxide solution i...

Embodiment 3

[0040] Put 1000g of o-cresol formaldehyde resin with a softening point of 100°C and 6000g of epichlorohydrin with a purity of 99.5% into the reaction vessel, so that the system material is under the protection of nitrogen with a purity (weight) of 99.5%, and the temperature is controlled at 80-100%. Dissolve at 82°C for 60 minutes to form a uniform transparent liquid, then control the reaction system at a vacuum of 0.078-0.082MPa, a temperature of 75±2°C, and a reflux rate of epichlorohydrin of 1200-1300g / h, and add the weight all at once Concentration 50% benzyltriethylammonium bromide and the dipropylene glycol solution 10g of triphenylethylammonium iodide mixture, after keeping 20 minutes, in the system, drip the NaOH aqueous solution 850g of weight concentration 49% again, dropwise During the process, keep the vacuum degree at 0.078-0.082MPa, the reaction temperature at 75±2°C, adjust and control the reflux flow at about 1200-1300g / h to carry out the water separation and cy...

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Abstract

The invention discloses a method for synthesizing phenol formaldehyde epoxy resin with (alkyl)phenolic resin and epoxy chloropropane as raw materials. Base resin and epoxy chloropropane undergo epoxidation reaction under the existence of catalyzer and alkali, and then are refined and processed with post treatment; in this way, phenol formaldehyde epoxy resin can be prepared. The epoxidation technique applied by the invention can effectively reduce the occurrence of side reaction and reduce production of isomerized chlorine and is easy to produce the products with high softening point, high epoxy equivalent weight and low chlorine content and has remarkable effects in improving the stability and heat resistance of the product and in reducing the consumption of the raw materials.

Description

technical field [0001] The invention relates to a preparation method for synthesizing a phenol-formaldehyde type epoxy resin with (alkyl) phenolic resin and epichlorohydrin as raw materials, in particular to an epoxidation method therein. Background technique [0002] (Alkyl) phenol formaldehyde type epoxy resin is obtained by condensation of phenol and aldehyde under the action of an acidic catalyst to obtain a thermoplastic linear base resin - (alkyl) phenolic resin, the (alkyl) phenolic resin and epoxy chlorine Propane undergoes epoxidation reaction, and then undergoes refining and post-treatment to obtain novolac epoxy resin. The product molecule contains two or more epoxy groups, and after curing, it will form a rigid and compact body structure with many cross-linking points. The cured product has high thermal stability and mechanical strength, excellent corrosion resistance, electrical insulation, water and solvent resistance, dimensional stability and other propertie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/08
Inventor 蒲建光宋尚林王平
Owner ZHONGHAO CHENGUANG RES INST OF CHEMICALINDUSTRY CO LTD
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