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Bisphenol A epoxy resin preparation method and product prepared therethrough

A technology of epoxy resin and bisphenol, which is applied in the field of preparation of bisphenol A epoxy resin, can solve problems such as high organic chlorine content, low softening point, and unclear process parameters, and achieve high epoxy value and softening point High, good process stability

Active Publication Date: 2015-03-25
建滔(广州)电子材料制造有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the bisphenol A type liquid epoxy resin prepared by this method has high purity, its organic chlorine content is high, the softening point is low, and the process parameters are not clear

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The preparation method of embodiment 1, bisphenol A type epoxy resin is as follows:

[0022] Add 10 mol of bisphenol A and 50 mol of epichlorohydrin into the reactor, and stir to dissolve them completely under the protection of nitrogen; then add 53 g of 45 wt% sodium hydroxide solution to the reactor, and react at a temperature of 58°C for 2 hours. After the pre-reaction is completed, vacuumize to 20kPa, add 1324g 45wt% sodium hydroxide solution dropwise at a temperature of 60°C, control the dropping rate of the sodium hydroxide solution to 0.4mL / min, and the alkali dropping time is 2.6h. After the ring-closing reaction is completed, the crude bisphenol A epoxy resin is obtained. After the ring-closing reaction, keep the vacuum of the reactor at 20kPa, increase the temperature to 80°C, and stir for 35 minutes; React for 35 minutes; in the second stage, reduce the vacuum of the reactor to 3kPa, increase the temperature to 122°C, and stir for 35 minutes. Add 4kg of tol...

Embodiment 2

[0023] The preparation method of embodiment 2, bisphenol A type epoxy resin is as follows:

[0024]Add 10 mol of bisphenol A and 60 mol of epichlorohydrin into the reactor, and stir to dissolve them completely under the protection of nitrogen; then add 80 g of 50 wt% sodium hydroxide solution to the reactor, and react at a temperature of 62°C for 3 hours. After the pre-reaction is completed, vacuumize to 25kPa, add 1512g of 50wt% sodium hydroxide solution dropwise at a temperature of 65°C, control the dropping rate of the sodium hydroxide solution to 0.8mL / min, and the alkali dropping time to 2.2h. After the ring-closing reaction is completed, the crude bisphenol A epoxy resin is obtained. After the ring-closing reaction, keep the vacuum of the reactor at 25kPa, increase the temperature to 75°C, and stir for 45 minutes; React for 45 minutes; in the second stage, reduce the vacuum of the reactor to 3kPa, increase the temperature to 118°C, and stir for 45 minutes. Add 4kg of ...

Embodiment 3

[0025] The preparation method of embodiment 3, bisphenol A type epoxy resin is as follows:

[0026] Add 10 mol of bisphenol A and 55 mol of epichlorohydrin into the reactor, and stir to dissolve them completely under the protection of nitrogen; then add 65 g of 49 wt% sodium hydroxide solution into the reactor, and react at a temperature of 60°C for 2.5 hours. After the pre-reaction is completed, vacuumize to 23kPa, add 1371g of 49wt% sodium hydroxide solution dropwise at a temperature of 64°C, control the dropping rate of the sodium hydroxide solution to 0.6mL / min, and the alkali dropping time to 2.4h. After the ring-closing reaction is completed, the crude bisphenol A epoxy resin is obtained. After the ring-closing reaction, keep the vacuum of the reactor at 23kPa, increase the temperature to 78°C, and stir for 40 minutes; React for 40 minutes; in the second stage, reduce the vacuum of the reactor to 4kPa, increase the temperature to 120°C, and stir for 40 minutes. Add 4k...

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Abstract

The invention discloses a bisphenol A epoxy resin preparation method and a product prepared therethrough. The method comprises the following steps: carrying out a pre-reaction and a ring closing reaction on raw materials comprising bisphenol A and chloropropylene oxide to prepare a crude bisphenol A epoxy resin, removing water and excess chloropropylene oxide, refining, desalinating, neutralizing through water washing, removing a solvent, and concentrating to obtain a bisphenol A epoxy resin. The preparation method has the advantages of stable process, clear parameters, detailed steps and strong feasibility; and the bisphenol A epoxy resin prepared through the preparation method has high purity, has an organic chloride content of below 0.02wt%, and has high epoxy value, high softening point and extremely good quality, so the performances of the bisphenol A epoxy resin are improved.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a preparation method of a bisphenol A epoxy resin and a prepared product thereof. Background technique [0002] Bisphenol A epoxy resin is also known as bisphenol A glycidyl ether epoxy resin, because of its good thermal stability, insulation, adhesion, corrosion resistance and other performance advantages, it is widely used in Coatings, adhesives, FRP, laminates, electronic casting, potting, encapsulation and other fields have become one of the most important electronic chemical materials. Bisphenol A epoxy resin is also the most widely used and the largest output in epoxy resin because of its convenient source of raw materials and low cost, accounting for more than 85% of the total output of epoxy resin. With the gradual expansion of the application of epoxy resin in high-tech fields, more stringent requirements are put forward for the heat resistance, mo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06
Inventor 张广军
Owner 建滔(广州)电子材料制造有限公司
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