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Synthesis method of four-functional group epoxy resin and prepared epoxy resin

A technology of agglomerated epoxy resin and synthesis method, applied in organic chemistry and other directions, can solve the problems of affecting performance and use, low epoxy value of epoxy resin, etc., to improve recovery rate, increase epoxy value, and reduce waste water production. Effect

Active Publication Date: 2010-06-16
建滔覆铜板(深圳)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the existing public documents, some preparation methods are improved by the manufacturing process of bisphenol A epoxy resin, such as step-by-step alkali addition method and vacuum alkali addition method, etc. It is difficult to avoid further condensation of the generated epoxy groups, resulting in low epoxy value of the synthesized epoxy resin, which seriously affects its performance and use

Method used

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  • Synthesis method of four-functional group epoxy resin and prepared epoxy resin
  • Synthesis method of four-functional group epoxy resin and prepared epoxy resin
  • Synthesis method of four-functional group epoxy resin and prepared epoxy resin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 199g (grams) of phenolic resin, 955g of epichlorohydrin, and 1.0g of tetraethylammonium bromide into a four-necked flask with a volume of 2000mL (milliliters) equipped with a stirring, heating and condensing device, and raise the temperature to 105-110°C , Reflux reaction for 4h for etherification reaction. After the reaction was completed, the temperature was lowered to 40°C, and 174 g of a metered sodium hydroxide aqueous solution with a mass fraction of 48.36% was added dropwise within 2.5 hours to carry out the ring-closing reaction, and the alkali was added to complete the heat preservation reaction for 4 hours. After the reaction is over, use dilute phosphoric acid solution to neutralize to a pH of 7.0-7.5 under stirring conditions, then stand still to separate the liquid to remove the water layer, and the resin layer is decompressed to recover epichlorohydrin and a small amount of water. The conditions for vacuum distillation are: The temperature is 140°C, th...

Embodiment 2

[0035] Synthetic condition is the same as embodiment 1, but adopts to blow into CO in neutralization step 2 to complete neutralization.

Embodiment 3

[0037] The synthesis conditions are the same as in Example 1, but deionized water is used for washing-layering-standstill-water removal process, and the washing process is carried out at least three times so that the pH of the resin system is close to 7.0-7.5.

[0038] Comparative Example 1'

[0039] The synthesis conditions are the same as in Example 1, but there is no neutralization step, and subsequent steps such as epichlorohydrin removal are directly carried out.

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Abstract

The invention discloses a synthesis method of four-functional group epoxy resin. The method comprises the following steps: 1. dissolving tetraphenolichydroxyl phenolic resin with epichlorohydrin, performing an etherification reaction under the existence of a catalyst; 2. adding excessive alkali to complete a ring-closure reaction; 3. blasting acidic gas or adding inorganic acid or adding water-soluble organic acid to neutralize and remove residual alkali, rinsing to remove salt, recycling epichlorohydrin to obtain four-functional group epoxy resin coarse product; and 4. refining the coarse product to obtain four-functional group epoxy resin. The invention also provides the epoxy resin prepared by the synthesis method. Compared with the synthesis method of four-functional group epoxy resin in the prior art, the epoxy value of the four-functional group epoxy resin of the invention is higher, the organochlorine content is low and the demand of the copper-clad plate on epoxy resin can be satisfied; and by using the synthesis method of the invention, the wastewater generated in the synthesis process is greatly reduced.

Description

technical field [0001] The invention relates to a method for synthesizing a four-functional epoxy resin and the epoxy resin prepared therefrom, belonging to the field of epoxy resin synthesis. Background technique [0002] The chemical name of the four-functional epoxy resin is 1,1,2,2-tetra(p-hydroxyphenyl)ethane tetraglycidyl ether, and its cured product has good thermochemical stability. For example, after curing with 4,4'-diaminodiphenyl sulfone (DDS), the shear strength can reach 10MPa at 250°C, while the shear strength of bisphenol A epoxy resin is close to zero under the same conditions. Therefore the resin can be used in adhesives, powder coatings, insulating laminates and aerospace composites. The molecular structure of the four-functional epoxy resin is a large π-bond delocalized structure containing multiple benzene nuclei, so that the entire molecular system has low energy and good stability. When irradiated by ultraviolet rays, the structure can absorb most of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/26C07D303/16C08G59/32
Inventor 张兴宏张国强闵玉勤张久久周国荣戚国荣
Owner 建滔覆铜板(深圳)有限公司
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