A kind of preparation method of bisphenol monomer containing phthalazinone structure

A technology of phthalazinone and monomers, which is applied in the field of preparation of bisphenol monomers containing phthalazinone structures, can solve problems such as poor solubility, and achieve the effects of mild reaction, reduced synthesis cost, and low raw material cost

Active Publication Date: 2022-06-14
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Traditional polyarylether materials, such as polyarylether ketone materials, are semi-crystalline polymers with excellent chemical stability and mechanical properties, but poor solubility, and are only soluble in concentrated sulfuric acid at room temperature

Method used

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  • A kind of preparation method of bisphenol monomer containing phthalazinone structure
  • A kind of preparation method of bisphenol monomer containing phthalazinone structure
  • A kind of preparation method of bisphenol monomer containing phthalazinone structure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: add DHPZ and K to the there-necked flask equipped with magnetic stirring, reflux condensing device 2 CO 3 , at 135 ° C for 5-6 hours of salt formation reaction, after the salt formation reaction is over, the reaction solution is lowered to room temperature, then Ullman coupling ligand PNTM, catalyst CuI and reactant BPM are added, and the reaction is protected from light for 12 hours. The temperature was gradually raised from room temperature to 130°C. After the reaction is completed, the reaction solution is immersed in hot water, drained overnight, the brown solid is dissolved in chloroform, the filtrate obtained by suction filtration is added with excess anhydrous sodium sulfate to remove water, and the brown powdery solid is obtained after rotary evaporation, using acetone or ethanol. Rinse 1-2 times to obtain a light yellow solid, which is vacuum dried in a vacuum drying oven at 100°C for 10-12 hours. Refined with DMAc at a mass-volume ratio of 1:2....

Embodiment 2

[0019] Embodiment 2: add DHPZ and K to the there-necked flask equipped with magnetic stirring, reflux condensing device 2 CO 3 , at 135 ℃ for 5-6 hours of salt formation reaction, after the salt formation reaction is over, the reaction solution is lowered to room temperature, then Ullman coupling ligand PNTM, catalyst CuI and reactant BPM are added, and the reaction is protected from light for 18 hours. The temperature was gradually raised from room temperature to 130°C. After the reaction is completed, the reaction solution is immersed in hot water, drained overnight, the brown solid is dissolved in chloroform, the filtrate obtained by suction filtration is added with excess anhydrous sodium sulfate to remove water, and the brown powdery solid is obtained after rotary evaporation, using acetone or ethanol. Rinse 1-2 times to obtain a light yellow solid, which is vacuum dried in a vacuum drying oven at 100°C for 10-12 hours. Refined with DMAc at a mass-volume ratio of 1:2.5 ...

Embodiment 3

[0020] Embodiment 3: add DHPZ and K to the there-necked flask equipped with magnetic stirring, reflux condensing device 2 CO 3 , at 135 ℃ for 5-6 hours of salt formation reaction, after the salt formation reaction is over, the reaction solution is lowered to room temperature, then Ullman coupling ligand PNTM, catalyst CuI and reactant BPM are added, and the reaction is darkened for 24 hours. The temperature was gradually raised from room temperature to 130°C. After the reaction is completed, the reaction solution is immersed in hot water, drained overnight, the brown solid is dissolved in chloroform, the filtrate obtained by suction filtration is added with excess anhydrous sodium sulfate to remove water, and the brown powdery solid is obtained after rotary evaporation, using acetone or ethanol. Rinse 1-2 times to obtain a light yellow solid, which is vacuum dried in a vacuum drying oven at 100°C for 10-12 hours. Refined with DMAc at a mass-volume ratio of 1:2.5 to obtain a ...

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Abstract

The invention discloses a preparation method of a bisphenol monomer containing a phthalazinone structure, belonging to the technical field of new materials. The bisphenol monomer containing phthalazinone structure in the present invention is synthesized by two-step reaction. Using bisphenol-like monomers containing phthalazinone structure and p-bromoanisole as raw materials, using 1,10-phenanthroline as N-N bidentate ligand, CuI as catalyst, through the first step The intermediate product DMPPZ was obtained after C‑O, C‑N Ullmann coupling reaction, and the target monomer DHPPZ was obtained by Lewis acid reduction. The synthesis reaction conditions provided by this patent have the advantages of short synthesis cycle and mild conditions. The purity of the target monomer was tested by liquid mass spectrometry to be 98%, and the yield was 85%-90%.

Description

technical field [0001] The invention belongs to the technical field of new materials, and relates to a preparation method of a bisphenol monomer (DHPPZ) containing a naphthalenone structure. Background technique [0002] The bisphenol monomer prepared and synthesized by the patent can be widely used in the synthesis of polyarylene ether materials, and the ether bond in the bisphenol monomer can increase the ductility and flexibility of the polyarylene ether materials. Traditional polyarylene ether materials, such as polyarylene ether ketone materials, are semi-crystalline polymers with excellent chemical stability and mechanical properties, but poor solubility, only soluble in concentrated sulfuric acid at room temperature. The bisphenol monomer has a novel fully aromatic ring, twisted, non-coplanar naphthylene ring structure, which can endow the polymer with outstanding heat resistance and solubility. Bisphenol monomers have good reactivity, have various reaction possibili...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D237/32
Inventor 蹇锡高王锦艳翁志焕刘程宗立率李楠
Owner DALIAN UNIV OF TECH
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