Synthetic method for bisphenol S epoxy resin

A technology of epoxy resin and synthesis method, applied in the field of synthesis of bisphenol S epoxy resin, can solve the problems of high reaction temperature, prolonged reaction time, affecting work efficiency, etc., and achieves lower reaction temperature, shortened reaction time, and improved work efficiency. The effect of efficiency

Inactive Publication Date: 2016-01-20
NANTONG BOTAO CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

RainerE, UdoG, HeinrichHW, etc. synthesized bisphenol S epoxy resin in a two-step method. The process is complex and requires multiple experiments, which increases the workload of the experiment.
The bisphenol S epoxy resin synthesized by SykoraV, SpacekV.J.Appl has low epoxy value, which affects the application of bisphenol S bonding performance
[0003] In view of the above phenomenon, the following two methods are available: (1) use alkali as a catalyst and directly synthesize bisphenol S epoxy resin by one-step precipitation method. The bisphenol S epoxy resin obtained by this synthesis method has good chemical stability and thermal stability. Yes, it has good bonding performance, but the reaction conditions of this method are not easy to control; (2) One-step synthesis of bisphenol S epoxy resin with phase transfer catalyst, the process is simple, the synthesized product has high purity and less impurities, and the epoxy value High, but the tetramethylammonium bromide used in this method has a melting point > 300 ° C, which makes the reaction temperature during the reaction very high and the reaction time is prolonged, thus affecting work efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The synthetic method of bisphenol S epoxy resin of the present embodiment, synthesizes bisphenol S epoxy resin by phase transfer catalyst one-step method, and the specific steps of this synthetic method are as follows:

[0015] (1) Feeding: Add a certain amount of 125g of bisphenol S, 700g of epichlorohydrin and 3g of tetrabutylammonium bromide into a four-necked flask equipped with a stirring paddle, a thermometer and a condenser, and mix and stir evenly in the four-necked flask , then dropwise add the catalyst sodium hydroxide that accounts for 2% of raw material total amount in flask;

[0016] (2) Control the reaction conditions: raise the temperature to 80°C to carry out the synthesis reaction, and react for 1 hour;

[0017] (3) Synthetic product: after the above reaction, the reactant solution was left at room temperature for 20 hours to obtain 795 g of a white precipitated product.

Embodiment 2

[0019] The synthetic method of bisphenol S epoxy resin of the present embodiment, synthesizes bisphenol S epoxy resin by phase transfer catalyst one-step method, and the specific steps of this synthetic method are as follows:

[0020] (1) Feeding: Add a certain amount of 125g of bisphenol S, 700g of epichlorohydrin and 5g of tetrabutylammonium bromide into a four-necked flask equipped with a stirring paddle, a thermometer and a condenser, and mix and stir evenly in the four-necked flask , then dropwise add the catalyst potassium hydroxide that accounts for 5% of raw material total amount in flask;

[0021] (2) Control the reaction conditions: raise the temperature to 100°C for the synthesis reaction, and react for 4 hours;

[0022] (3) Synthetic product: After the above reaction, the reactant solution was left at room temperature for 24 hours to obtain 790 g of a white precipitated product.

Embodiment 3

[0024] The synthetic method of bisphenol S epoxy resin of the present embodiment, synthesizes bisphenol S epoxy resin by phase transfer catalyst one-step method, and the specific steps of this synthetic method are as follows:

[0025] (1) Feeding: Add a certain amount of 125g of bisphenol S, 700g of epichlorohydrin and 5g of tetrabutylammonium bromide into a four-necked flask equipped with a stirring paddle, a thermometer and a condenser, and mix and stir evenly in the four-necked flask , then in the flask, dropwise add the catalyst triethylamine that accounts for 3% of raw material total amount;

[0026] (2) Control the reaction conditions: raise the temperature to 90°C for the synthesis reaction, and react for 2.5 hours;

[0027] (3) Synthesized product: after the above reaction, the reactant solution was left at room temperature for 22 hours to obtain 810 g of a white precipitated product.

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Abstract

The invention relates to a synthetic method for bisphenol S epoxy resin. The bisphenol S epoxy resin is synthesized through a phase transfer catalyst one-step method. The method comprises the following steps of throwing materials, wherein a certain amount of bisphenol S, a certain amount of epichlorohydrin and a certain amount of tetrabutylammonium bromide are added into a four-necked flask provided with a stirring paddle, a thermometer and a condenser pipe, and a catalyst accounting for 2-5% of the total amount of the raw materials is dripped into the flask; controlling reaction conditions, wherein temperature is raised to 80 DEG C-100 DEG C, and a synthetic reaction is carried out for 1-4 h; synthesizing a product, wherein after the reaction is finished, a reactant solution is placed for 20-24 h at the normal temperature to obtain a white precipitate product. The synthetic method has the advantages that tetramethylammonium bromide is replaced by tetrabutylammonium bromide, the melting point of tetrabutylammonium bromide is 100 DEG C-104 DEG C, the reaction temperature falls relatively, the reaction time is shortened, and the working efficiency is improved; meanwhile, the product yield of the synthetic method is high, and an epoxy value is large.

Description

technical field [0001] The invention relates to the field of organic compound synthesis, in particular to a method for synthesizing bisphenol S epoxy resin. Background technique [0002] Bisphenol S epoxy resin is a new type of epoxy resin, due to the introduction of -SO 2 - Polar groups, so it has better flexibility, compressive strength and thermal stability than traditional bisphenol A epoxy resins. Its glass transition temperature is more than 40°C higher than that of bisphenol A epoxy resin system under the same curing conditions. With the rapid expansion of the application of polymer materials, there are more and more researches on bisphenol S epoxy resin. RainerE, UdoG, HeinrichHW, etc. synthesized bisphenol S epoxy resin with a two-step method. The process is complex and requires multiple experiments, which increases the workload of the experiment. The bisphenol S epoxy resin synthesized by SykoraV, SpacekV.J.Appl has low epoxy value, which affects the application...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/06
Inventor 黄海涛王宏李桂萍
Owner NANTONG BOTAO CHEM
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