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A kind of preparation method of high molecular weight phenoxy resin

A phenoxy resin and high-molecular-weight technology, which is applied in the field of preparation of high-molecular-weight phenoxy resin, can solve problems such as high water content in products, affecting product performance, and difficulty in dehydration, so as to achieve easy control of reactions, less raw material residues, and product color. good effect

Active Publication Date: 2019-04-05
辽阳鑫宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Patent CN95114257.7 discloses a process for synthesizing polyphenolic resin (phenoxy resin) by dispersion polycondensation method. Due to the reaction under aqueous conditions, a large amount of basic catalyst needs to be added, the reactants are not uniformly dispersed, and the molecular weight of the product is dispersed. Affect product performance; there are production problems such as high water content in the product, difficulty in dehydration, and inability to monitor the molecular weight of the product during the reaction process

Method used

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  • A kind of preparation method of high molecular weight phenoxy resin
  • A kind of preparation method of high molecular weight phenoxy resin
  • A kind of preparation method of high molecular weight phenoxy resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The preparation method of the high molecular weight phenoxy resin of the present embodiment is carried out according to the following steps:

[0032] (1) In a 2000Ml glass-made 4-port detachable flask experimental device equipped with a stirring device, a thermometer, a condenser, and a nitrogen inlet pipe, 55 parts of liquid bisphenol A type 128 epoxy resin, 195 parts of bisphenol A type 604 Solid epoxy resin and 65 parts of bisphenol A are used as raw materials. Under the condition of nitrogen protection, the raw materials are dissolved in 160ml of MIBK solvent at 80°C, and 4 parts of 40% KOH solution of basic catalyst are added, and the reaction is carried out at 90°C for 5 hours. During the reaction, the solvent was added every 30 minutes. The total amount of added solvent was 3 times the weight of the solvent when feeding. Gel permeation chromatography was used to detect the molecular weight of the reaction product in real time. After the molecular weight reached 70...

Embodiment 2

[0035] The preparation method of the high molecular weight phenoxy resin of the present embodiment is carried out according to the following steps:

[0036] (1) In a 2000Ml glass-made 4-port detachable flask experimental device equipped with a stirring device, a thermometer, a condenser, and a nitrogen inlet pipe, 55 parts of liquid bisphenol A type 128 epoxy resin, 195 parts of bisphenol A type 604 Solid epoxy resin and 65 parts of bisphenol A are used as raw materials, and the raw materials are dissolved in 160ml of toluene and butanol mixed solvent at 85°C under the condition of nitrogen protection, and 4 parts of 40% KOH solution of basic catalyst are added. React for 6 hours. During the reaction, add a solvent every 30 minutes. The total amount of added solvent is 4 times the weight of the solvent when feeding. Use gel permeation chromatography to detect the molecular weight of the reaction product in real time. After the molecular weight reaches 70,000 Phosphoric acid wa...

Embodiment 3

[0039] The preparation method of the high molecular weight phenoxy resin of the present embodiment is carried out according to the following steps:

[0040] (1) In a 2000Ml glass-made 4-port detachable flask experimental device equipped with a stirring device, a thermometer, a condenser, and a nitrogen inlet pipe, 55 parts of liquid bisphenol A type 128 epoxy resin, 195 parts of bisphenol A type 604 Solid epoxy resin and 57 parts of bisphenol F are used as raw materials. Dissolve the raw materials in 160ml of MIBK solvent at 90°C under nitrogen protection, add 4 parts of 40% KOH solution of basic catalyst, and react at 90°C for 5 hours. During the reaction, add a solvent every 30min, the added total amount of the added solvent is 3 times of the solvent weight when feeding, adopt gel permeation chromatography to detect the molecular weight of the reaction product in real time, add phosphoric acid after the molecular weight reaches 70000, stop reaction;

[0041] (2) Wash the mi...

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Abstract

The invention belongs to the technical field of preparation of epoxy resin, and particularly relates to a method for preparing high-molecular-weight phenoxy resin. According to the method, the phenoxy resin with the weight average molecular weight being 50,000 to 80,000 is prepared through the steps of raw material ratio control, proper solvent and catalyst selection, nitrogen introduction in the whole reaction process for protection and reaction product molecular weight real-time detection through a gel permeation chromatograph. According to the method, few by-products are generated in the reaction process, the reaction is easy to control, few raw material residues are generated in the product, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of epoxy resin preparation, and in particular relates to a preparation method of high molecular weight phenoxy resin. Background technique [0002] Epoxy resins are widely used in the fields of electronic parts, electrical equipment, automotive parts, and sporting goods due to their excellent adhesiveness, heat resistance, and formability. Especially in recent years, epoxy resin is one of the materials attracting much attention in the field of electronic materials. [0003] The earliest application of phenoxy resin was as an engineering plastic. It is a nearly colorless to light yellow transparent plastic. Due to the presence of benzene rings and hydroxyl groups in the main molecular chain, it has excellent mechanical strength and toughness. It can still show good ductility, low creep and mold shrinkage at high loading speeds, and it has good mechanical properties, electrical properties and creep resistance...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/40C08G59/20
CPCC08G59/20C08G65/40
Inventor 郭树志
Owner 辽阳鑫宇化工有限公司
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