Method for preparing fluorine-containing epoxy resin by phase transfer catalyst

Abstract

The invention relates to a method for preparing fluorine-containing epoxy resin by a phase transfer catalyst, which is characterized by comprising the following steps: 1) etherification: selecting raw materials according to the mol ratio of fluorine-containing monomer and epoxy chloropropane being 1:1-10 and the addition of phase transfer catalyst being 0.5-2% of the fluorine-containing monomer mol; adding fluorine-containing monomer, epoxy chloropropane, phase transfer catalyst and water into a reactor for reaction for 0.5-3h within the temperature range of 65-80 DEG C to obtain etherification reaction liquid; 2) ring-closing reaction: dripping alkaline solution accounting for 50-80% of the total amount of the alkaline solution for reaction for 1-5h within the temperature range of 65-80 DEG C; reduced pressure distilling un-reacted epoxy chloropropane, cooling the temperature below 65 DEG C, adding an organic solvent, then dripping the residual alkaline solution and refluxing for 1-3h; and 3) purifying to obtain the fluorine-containing epoxy resin. The fluorine-containing epoxy resin prepared in the invention has the epoxy value (eq / 100g) range of 0.09-0.57, and the method reduces the unit consumption of epoxy chloropropane and has the advantages of little solvent discharge, high yield, little energy consumption, stable parameter and the like.

Description

technical field [0001] The invention belongs to the field of polymer preparation, and in particular relates to a preparation method of fluorine-containing epoxy resin. Background technique [0002] Phase transfer catalysis is a new synthesis method developed after the 1970s. The method of phase transfer can realize many reactions that cannot be completed by traditional synthetic methods, and has high yield, mild reaction conditions and easy handling of products. So far, phase transfer catalysis has been widely used in various types of organic synthesis such as carbonylation, acylation, cyanation and coupling (Su Biquan, Phase transfer catalysts in organic synthesis, Lanzhou Jiaotong University, 200306 (67-68)). The preparation of fluorine-containing epoxy resin with hexafluorobisphenol A was first reported by the United States, and domestic people also used a one-step method to directly use alkali as a catalyst to prepare fluorine-containing epoxy resin (Shan Songgao, Synt...

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Problems solved by technology

The preparation of fluorine-containing epoxy resin with hexafluorobisphenol A was first reported by the United States, and domestic people also used a one-step method to directly use alkali as a catalyst to prepare fluorine-containing epoxy resin (Shan Songgao, Synthesis of fluorine-containing epoxy resin, Wuhan Industry University, 199503 (50-51)), but in the process of directly using alkali as a catalyst to prepare fluorine-containing epoxy resin, the solvent emission is large, the yield is low, and the energy consumption is high, resulting in a large range of product molecular weight distribution and unstable parameters

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