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A kind of high-purity bisphenol A type liquid epoxy resin production process

A technology of liquid epoxy resin and production process, applied in the field of epoxy resin production, can solve problems such as quality degradation, unfavorable environmental protection, and increase of intermediate processing cost, etc.

Active Publication Date: 2021-06-08
南亚电子材料(昆山)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of high-purity bisphenol A type liquid epoxy resin production process, solve the process of the production of existing epoxy resin, the purity of reclaiming epichlorohydrin (ECH) is less than 99%, and moisture More than 0.5%, repeated use of the recycled epichlorohydrin (ECH) will lead to a decline in the quality of epoxy resin production, while epoxy resin and water are hydrolyzed under the action of NaOH, and the hydrolyzate is further polymerized in the reaction to produce Insoluble solid waste, this kind of solid waste needs to be disposed of by incineration and landfill, which increases the processing cost of intermediates and is not conducive to environmental protection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The recovered epichlorohydrin is purified by the reused epichlorohydrin purification tower, and the purity of epichlorohydrin is greater than 99.0%, and the moisture is less than 0.5%. The bottom product of the purification tower is epichlorohydrin hydrolyzate and its polymer.

[0032] Add 230.79g of bisphenol A, 187.27g of fresh ECH (epichlorohydrin), and 292.54g of purified ECH into a four-neck flask with stirring, thermometer, and condenser, at a temperature of 50°C and under the protection of high-purity nitrogen Add 15g of 48.5% sodium hydroxide solution for pre-reaction, after maintaining for 4 hours, dropwise add 132.7g of 48.5% sodium hydroxide solution under vacuum of 200 Torr to catalyze the ring-closure reaction, recover ECH after 5 hours of reaction, and then add 300g of toluene Dissolve, at a temperature of 65°C, add 1g of the hydrolyzate produced by purified epichlorohydrin and its polymer, add 13.1g of 48.5% sodium hydroxide solution to refine for 75 minu...

Embodiment 2

[0034] Embodiment 2, the difference between this embodiment and embodiment 1 is:

[0035] The recovered epichlorohydrin is purified by the reused epichlorohydrin purification tower, and the purity of epichlorohydrin is greater than 99.0%, and the moisture is less than 0.5%. The bottom product of the purification tower is epichlorohydrin hydrolyzate and its polymer.

[0036]Add 230.79g of bisphenol A, 187.27g of fresh ECH (epichlorohydrin), and 292.54g of purified ECH into a four-neck flask with stirring, thermometer, and condenser, at a temperature of 50°C and under the protection of high-purity nitrogen Add 15g of 48.5% sodium hydroxide solution for pre-reaction, after maintaining for 4 hours, dropwise add 132.7g of 48.5% sodium hydroxide solution under vacuum of 200 Torr to catalyze the ring-closure reaction, recover ECH after 5 hours of reaction, and then add 300g of toluene Dissolve, add 1g of purified epichlorohydrin hydrolyzate and its polymer at a temperature of 65°C, ...

Embodiment 3

[0038] Embodiment 3, the difference between this embodiment and embodiment 1, embodiment 2 is:

[0039] The recovered epichlorohydrin is purified by the reused epichlorohydrin purification tower, and the purity of epichlorohydrin is greater than 99.0%, and the moisture is less than 0.5%. The bottom product of the purification tower is epichlorohydrin hydrolyzate and its polymer.

[0040] Add 230.79g of bisphenol A, 187.27g of fresh ECH (epichlorohydrin), and 476.69g of purified ECH into a four-neck flask with stirring, thermometer, and condenser, at a temperature of 50°C and under the protection of high-purity nitrogen Add 15g of 48.5% sodium hydroxide solution for pre-reaction, after maintaining for 4 hours, dropwise add 133.5g of 48.5% sodium hydroxide solution under vacuum of 200 Torr for ring closure reaction, recover ECH after 5 hours of reaction, and then add 300g of toluene Dissolve, add 1.5g of epichlorohydrin hydrolyzate and its polymer at a temperature of 60°C, add ...

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Abstract

The invention discloses a production process of high-purity bisphenol A liquid epoxy resin, comprising the following steps: Step 1, the purification of epichlorohydrin recycled in the process and the application of its hydrolyzed polymer: adding recycled epoxy chlorine Propane purification tower, the purity of epichlorohydrin is more than 99.0%, and the water content is less than 0.5%. The purified epichlorohydrin is reused in the reaction section of epoxy resin, and the bottom product is epichlorohydrin hydrolysis product and its polymerization things. The purpose of the present invention is to provide high-purity epoxy resin and a preparation method of low-solid waste generation. This method adopts the reuse of purified epichlorohydrin to reduce the content of bishydroxyl resin and total chlorine in the epoxy resin, and it is recycled in the process of using The epichlorohydrin hydrolyzate and its polymer after epichlorohydrin purification are reused in the refining stage reaction. It has surface active properties, which can promote the full contact between the organic phase and the water, improve the efficiency of hydrolyzed chlorine ring closure, and reduce the residual hydrolyzed chlorine. And reduce the formation of intermediates.

Description

technical field [0001] The invention relates to the technical field of epoxy resin production, in particular to a production process of high-purity bisphenol A liquid epoxy resin. Background technique [0002] Epoxy resin generally refers to organic polymer compounds containing two or more epoxy groups in the molecule. Among them, liquid bisphenol A epoxy resin is the most basic general-purpose epoxy resin. It is compatible with various types of The curing agent undergoes cross-linking reaction, has excellent mechanical properties, adhesive properties, electrical insulation properties and chemical resistance properties, and has been widely used in composite materials, coatings, adhesives, copper clad laminates, civil engineering and other fields. [0003] The industrial production steps are: bisphenol A (BPA) and epichlorohydrin (ECH) are polymerized under the action of sodium hydroxide to generate epoxy resin and by-product NaCl. In order to control the molecular weight of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/06C08G59/02
CPCC08G59/025C08G59/063
Inventor 柯有明
Owner 南亚电子材料(昆山)有限公司