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A kind of synthetic method of bisphenol S derivative type polysulfate

A technology of polysulfate ester and synthesis method, which is applied in the field of polymer materials, can solve the problems of incomplete reaction of bisphenol S sulfonyl fluoride monomer, low dielectric loss, etc., achieve simple and stable synthesis process, and low orientation polarization temperature , is conducive to the effect of industrial production

Active Publication Date: 2022-05-06
内蒙古图微新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to provide a synthetic method of bisphenol S derivative type polysulfate, which solves the problem of incomplete reaction of bisphenol S sulfonyl fluoride monomer and the influence of impurities on polymerization in the later stage of polymerization, and the synthesis process is simple and stable , economical, recyclable by-products, less environmental pollution, high glass transition temperature, good electrical insulation and low dielectric loss, has broad application prospects in aviation, communications, electronics and microelectronics industries

Method used

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Embodiment 1

[0037] A kind of synthetic method of bisphenol S derivative type polysulfate, comprises the following steps:

[0038] 1. Preparation of 4,4-disulfonyl fluoride diphenyl sulfone

[0039] (1) First put 1000g of bisphenol S monomer in a 50L autoclave, with a purity of 99.5% or more; put in 20L of DCM, stir in the autoclave, and stir at room temperature; add 971g of triethylamine, the temperature is 25°C, and stir for 30min Finally, inject 960g of sulfuryl fluoride gas, and the reaction time is 13h.

[0040] (2) Rotate the mixture obtained in (1) under reduced pressure in a 35°C water bath, spin out the solvent DCM and recover it, add 490ml of methanol solution and 1225ml of water to the remaining system, heat to boil at 90°C and reflux, mechanically After stirring, the solid was filtered out to obtain the target product, and 1324 g of white powder was obtained.

[0041](3) The aqueous methanol solution obtained in (2) was distilled under reduced pressure in a water bath at 70°C...

Embodiment 2

[0046] 1. Preparation of 4,4-disulfonyl fluoride diphenyl sulfone

[0047] Preparation method is identical with embodiment 1

[0048] Two, the synthesis of bisphenol S derivative type polysulfate

[0049] (1) Weigh 1000g of bisphenol S, 1672.5g of 4,4-disulfonyl fluoride diphenyl sulfone, 493g of potassium hydroxide, and 16.13L of nitrobenzene solution, and add them to the polymerization kettle at one time and stir, and the temperature rises from room temperature to 50°C-150°C. The heating time is 2h, 6h, and 2h. After the reaction is completed, the material is discharged under pressure with nitrogen and settled in the ethanol solution.

[0050] (2) Put the polymer obtained in (1) into a 10L autoclave, add 5L of purified water, boil at 120°C for 5 hours, repeat once, after drying, use 6L methanol solution to boil once at 100°C, and dry. A bisphenol S derivative type polysulfate was obtained.

Embodiment 3

[0052] 1. Preparation of 4,4-disulfonyl fluoride diphenyl sulfone

[0053] Preparation method is identical with embodiment 1

[0054] Two, the synthesis of bisphenol S derivative type polysulfate

[0055] (1) Weigh 1000g of bisphenol S, 1689g of 4,4-disulfonyl fluoride diphenyl sulfone, 493g of potassium hydroxide, and 16.13L of nitrobenzene solution, add them into the polymerization kettle at one time and stir, and the temperature rises from room temperature to 50 ℃-150℃. The heating time is 2h, 6h, and 2h. After the reaction is completed, the material is discharged under pressure with nitrogen and settled in the ethanol solution.

[0056] (2) Put the polymer obtained in (1) into a 10L autoclave, add 5L of purified water, boil at 120°C for 5 hours, repeat once, after drying, use 6L methanol solution to boil once at 100°C, and dry , to obtain bisphenol S derivative polysulfate.

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Abstract

The invention discloses a method for synthesizing bisphenol S derivative type polysulfate, comprising the following steps: (1) adding catalyst triethylamine into dichloromethane in which bisphenol S derivatives are dissolved, stirring, and introducing sulfur Acyl fluoride gas to obtain disulfonyl fluoride diphenyl sulfone derivatives; (2) Purify disulfonyl fluoride diphenyl sulfone derivatives and recycle triethylamine; (3) In the presence of catalysts, bisphenol S derivatives and disulfone The sulfonyl fluoride diphenyl sulfone derivatives are polymerized at 50° C. to 150° C. to form bisphenol S derivative type polysulfate; (4) purifying the bisphenol S derivative type polysulfate. The synthesis process of the present invention solves the problem of incomplete reaction of bisphenol S sulfonyl fluoride monomer and the influence of impurities on the polymerization in the later stage of polymerization. Glass transition temperature, good electrical insulation and low dielectric loss, have broad application prospects in aviation, communication, electronics and microelectronics industries.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to a method for synthesizing bisphenol S derivative polysulfate. Background technique [0002] Fluorine sulfur exchange (SuFEx) click reaction is a new generation of click chemistry reported by Professor Sharpless in 2014. The system selects cheap industrial insecticide sulfuryl fluoride (SO2F2) and 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 chem...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G75/24
CPCC08G75/24
Inventor 梁鹏强周云斌
Owner 内蒙古图微新材料科技有限公司
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