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

A phase transfer catalyst and fluorine-containing epoxy resin technology, applied in the field of polymer preparation, can solve the problems of large molecular weight distribution range, large solvent discharge, unstable parameters, etc., and achieve stable product parameters, less solvent discharge, and reduced Single consumption effect

Inactive Publication Date: 2009-12-30
WUHAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 I

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0020] A kind of phase transfer catalyst prepares the method for fluorine-containing epoxy resin, such as figure 1 As shown, it includes the following steps:

[0021] 1) etherification reaction: choose 1mol of hexafluorobisphenol A (bisphenol AF), 10mol of newly steamed epichlorohydrin, 0.01mol of tetramethylammonium chloride, 10mol of distilled water; mix hexafluorobisphenol A, Add epichlorohydrin, tetramethylammonium chloride and distilled water into a four-necked bottle or reaction kettle equipped with a stirrer, a thermometer, a condenser and a dropping funnel, raise the temperature to 70°C, and react for 2 hours to obtain an etherification reaction liquid;

[0022] 2) ring-closing reaction: by the mole of the sodium hydroxide in the sodium hydroxide solution is 4mol, choose the sodium hydroxide solution that mass fraction is 20% (that is, contain 20g sodium hydroxide in the 100g sodium hydroxide solution); Choose the benzene of 3mol ; In the etherification reaction solu...

Embodiment 2

[0025] A kind of method that phase-transfer catalyst prepares fluorine-containing epoxy resin, it comprises the steps to carry out:

[0026] 1) etherification reaction: choose 1mol of hexafluorobisphenol A (bisphenol AF), 1mol of newly steamed epichlorohydrin, 0.005mol of tetraethylammonium chloride, 10mol of distilled water; mix hexafluorobisphenol A, Add epichlorohydrin, tetraethylammonium chloride and distilled water into a four-necked bottle or reactor equipped with a stirrer, a thermometer, a condenser and a dropping funnel, raise the temperature to 80°C, and react for 0.5 hours to obtain an etherification reaction liquid;

[0027] 2) ring-closing reaction: by the mole of the sodium hydroxide in the sodium hydroxide solution is 4mol, choose the sodium hydroxide solution that the mass fraction is 10%; Choose the toluene of 2mol; To the etherification reaction solution that step 1) obtains, add dropwise Sodium hydroxide solution with 50% of the total amount of sodium hydro...

Embodiment 3

[0030] A kind of method that phase-transfer catalyst prepares fluorine-containing epoxy resin, it comprises the steps to carry out:

[0031] 1) etherification reaction: choose 1mol of hexafluorobisphenol A (bisphenol AF), 1.4mol of newly steamed epichlorohydrin, 0.015mol of tetrabutylammonium chloride, 15mol of distilled water; , epichlorohydrin, tetrabutylammonium chloride and distilled water are added to a four-necked bottle or reactor equipped with a stirrer, thermometer, condenser and dropping funnel, heated to 65°C, and reacted for 2.5 hours to obtain etherification The reaction solution;

[0032] 2) ring-closing reaction: according to the mole of the potassium hydroxide in the potassium hydroxide solution is 5mol, choose the potassium hydroxide solution that mass fraction is 5%; Choose the xylene of 1mol; To step 1) drop in the etherification reaction liquid that obtains Add potassium hydroxide solution with 70% of the total amount of potassium hydroxide solution, react...

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PUM

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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...

Claims

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Application Information

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IPC IPC(8): C08G59/68C08G59/06
Inventor 易英黄畴饶建波官建国武娜
Owner WUHAN UNIV OF TECH
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