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Preparation method of polysulfate type epoxy resin

A polysulfate and epoxy resin technology, applied in the field of polymer materials, can solve problems such as mechanical property defects, and achieve the effects of simple and stable reaction process, less by-products, and less environmental pollution

Active Publication Date: 2022-01-14
BAIYIN TUWEI NEW MATERIALS TECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on the above, the purpose of the present invention is to provide a kind of preparation method of polysulfate type epoxy resin, to solve the defect of existing polysulfate ester in mechanical properties, and the obtained polysulfate type epoxy resin of this preparation method It can also be used in areas with high anti-corrosion requirements

Method used

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  • Preparation method of polysulfate type epoxy resin

Examples

Experimental program
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Embodiment 1

[0037] The preparation method of the polysulfate type epoxy resin provided by the present embodiment may further comprise the steps:

[0038] 1. Preparation of low molecular weight polysulfate

[0039] (1-1) First put 400g of bisphenol A, 300g of bisphenol A bissulfonyl fluoride, 1.2kg of sulfolane, and 250g of potassium carbonate into a 50L autoclave, and react at 170°C for 4h to prepare polysulfate.

[0040] (1-2) After the polysulfate was precipitated, it was boiled twice in ethanol at 100°C, and boiled in high-purity water three times at 140°C, filtered and dried at 80°C, and the number average molecular weight Mn=3562g / mol was measured.

[0041] 2. Preparation of Epoxy Resin

[0042] (2-1) Take 500 g of the treated bisphenol A polysulfate, add 2.5 kg of epichlorohydrin as a solvent, and heat and stir at 80° C. for 2 hours to fully dissolve the polysulfate.

[0043] (2-2) Add 15 g of ring-opening catalyst tetrabutylammonium bromide to the solution obtained in step (2-1),...

Embodiment 2

[0048] The preparation method of the polysulfate type epoxy resin provided by the present embodiment may further comprise the steps:

[0049] 1. the preparation of low molecular weight polysulfate, with embodiment 1

[0050] 2. Preparation of Epoxy Resin

[0051](2-1) Take 500 g of the treated bisphenol A polysulfate, add 3.0 kg of epichlorohydrin as a solvent, and heat and stir at 80° C. for 2 hours to fully dissolve the polysulfate.

[0052] (2-2) Add 15 g of tetrabutylammonium bromide, a ring-opening catalyst, to the solution obtained in step (2-1), and stir at 90° C. for 3 hours.

[0053] (2-3) Add ring-closing catalyst sodium hydroxide solution to the solution obtained in step (2-2) with stirring, the concentration of sodium hydroxide solution is 30wt%, and then stir and heat at 70° C. for 3 hours.

[0054] (2-4) Pour the solution obtained in step (2-3) into 5 L of methanol for sedimentation, and then take out the precipitate.

[0055] (2-5) Add the precipitate obtaine...

Embodiment 3

[0057] The preparation method of the polysulfate type epoxy resin provided by the present embodiment may further comprise the steps:

[0058] 1. the preparation of low molecular weight polysulfate, with embodiment 1

[0059] 2. Preparation of Epoxy Resin

[0060] (2-1) Take 500 g of the treated bisphenol A polysulfate, add 3.0 kg of epichlorohydrin as a solvent, and heat and stir at 80° C. for 2 hours to fully dissolve the polysulfate.

[0061] (2-2) Add 15 g of tetrabutylammonium bromide, a ring-opening catalyst, to the solution obtained in step (2-1), and stir at 90° C. for 3 hours.

[0062] (2-3) Add ring-closing catalyst sodium hydroxide solution with stirring to the solution obtained in step (2-2). The concentration of the sodium hydroxide solution is 20 wt%, and then stir and heat at 70° C. for 3 hours.

[0063] (2-4) Pour the solution obtained in step (2-3) into 5 L of methanol for sedimentation, and then take out the precipitate.

[0064] (2-5) Add the precipitate o...

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Abstract

The invention relates to a preparation method of polysulfate type epoxy resin. The preparation method comprises the steps of (1) preparing polysulfate of which the number-average molecular weight is 1000-10000 g / mol and the terminal group is hydroxyl; (2) heating and dissolving polysulfate in epoxy halopropane; (3) continuing to add a ring-opening catalyst, and enabling epoxy halopropane to react with polysulfate; (4) continuing to add a ring-closed catalyst, and enabling the end group of the polysulfate to be changed into an epoxy structure; and (5) separating out the product, and purifying. The preparation method provided by the invention can realize large-scale industrial production, and has the advantages of simple post-treatment process and small pollution.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a preparation method of polysulfate-type epoxy resin. Background technique [0002] Fluorine sulfur exchange (SuFEx) click reaction is a new generation of click chemistry reported by Professor Sharpless in 2014. The system uses cheap industrial insecticide sulfuryl fluoride (SO 2 f 2 ) react with phenolic compound to prepare the substrate of SuFEx click reaction. The synthetic polysulfate material has acid and alkali resistance, high glass transition temperature and excellent mechanical properties. [0003] High-valent main group fluorides have high chemical stability, but their activation under specific conditions can achieve extremely efficient chemical bond conversion and linkage. This special combination of stability and reactivity determines that this type of compound is in There will be unique potential applications in synthetic organic chemistry, materials ch...

Claims

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Application Information

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IPC IPC(8): C08G59/06
CPCC08G59/063
Inventor 刘江陈金炜周云斌
Owner BAIYIN TUWEI NEW MATERIALS TECHNOLOGY CO LTD
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