Bi(4-(4-fluorobenzoyl)phenyl)phenyl phosphine oxide monomer and synthetic method thereof

A technology of fluorobenzoyl and phenylphosphine oxide, applied in the field of novel structure phosphorus-containing aromatic difluoride monomer and its synthesis, can solve the problems of high melting temperature of polyaryl ether ketone, difficult processing, insoluble and the like , to achieve the effect of strong repeatability, high monomer yield and high purity

Inactive Publication Date: 2007-10-24
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Polyaryletherketone has a high melting temperature and is insoluble in general organic solvents, making it difficult to process

Method used

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  • Bi(4-(4-fluorobenzoyl)phenyl)phenyl phosphine oxide monomer and synthetic method thereof
  • Bi(4-(4-fluorobenzoyl)phenyl)phenyl phosphine oxide monomer and synthetic method thereof
  • Bi(4-(4-fluorobenzoyl)phenyl)phenyl phosphine oxide monomer and synthetic method thereof

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Experimental program
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Effect test

Embodiment 1

[0022] Embodiment 1: the synthesis of CPPPO involved in the present invention

[0023] Add 22.0g (0.06mol) BCPPO, 100ml thionyl chloride and 4-5 drops of catalyst DMF in a 250ml four-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, react at reflux temperature for 6h, and distill under reduced pressure Excessive thionyl chloride was removed, the residual thionyl chloride was washed with n-hexane, and vacuum-dried to obtain 22.8 g of light yellow solid CPPPO, with a yield of 94%.

Embodiment 2

[0024] Embodiment 2: the synthesis of FPPPO involved in the present invention

[0025] Add 24.5g (0.06mol) CPPPO, 24.0g (0.18mol) AlCl 3 and 60ml of dichloromethane, add 15ml (0.16mol) fluorobenzene dropwise with a constant pressure funnel at 40°C, react at this temperature for 5 hours, pour the reactant into 200ml of water to remove AlCl 3 , suction filtration, then the solid product is poured into 200ml 10% sodium hydroxide solution to remove the acidic substance remaining in the product, and the product is washed to neutrality with distilled water, and suction filtration obtains 27.2g light yellow powdery crystals, producing The rate is 86%.

Embodiment 3

[0026] Embodiment 3: the purification of FPPPO involved in the present invention

[0027] Add 25.0g of FPPPO, 75ml of DMF, 250ml of absolute ethanol into a 500ml four-neck flask equipped with a magnetic stirrer, a thermometer and a reflux condenser, add 0.75g of activated carbon, reflux for 60min, and suction filter while it is hot to obtain a light yellow solution. After natural cooling and static crystallization, 22.6 g of white powder crystal FPPPO was obtained by filtration.

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Abstract

The invention discloses a new aromatic bifluoride monomer with phosphor and compounding and purifying technique with structure as formula (I), which comprises the following steps: affirming the polymer as object product through infrared spectrum and nuclear magnetic resonance; adopting BCPPO and sulfone chloride as raw material; acylating and chlorinating to obtain CPPPO; reacting the CPPPO and fluorobenzene; making anhydrous aluminium trichloride as catalyst to synthesize the FPPPO through Friedel-Crafts reaction.

Description

technical field [0001] The invention belongs to the field of polymer materials and their preparation, and in particular relates to a novel structure phosphorus-containing aromatic difluoride monomer and its synthesis technology. Background technique [0002] Polyaryletherketone has excellent thermal properties, mechanical properties, electrical insulation properties and chemical resistance, and is widely used in aerospace, electronic appliances, nuclear energy industry and civil high-tech fields. Polyaryletherketone has a high melting temperature and is insoluble in general organic solvents, making it difficult to process. In order to improve the solubility and processability of polyaryletherketone, large side groups, flexible groups, twisted non-planar structures or copolymerization methods can be introduced into the main chain. Synthesized a kind of heterocyclic compound-4,4-diphenyl-2,3-diazinone-1 (DHPZ) with similar bisphenol structure as Hay et al., and difluorobenzop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/53
Inventor 唐旭东陈晓婷孙皓张明珠贺征华王春颖
Owner TIANJIN UNIV OF SCI & TECH
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