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Method for synthesizing polymerized phenyl phosphonate by performing solid-liquid two-phase reaction

A phenylphosphonate, polymerized technology, applied in the field of solid-liquid two-phase reaction synthesis of polymerized phenylphosphonates, can solve the problems of high volatility, decreased physical properties, poor heat resistance, etc., and achieves a high degree of polymerization. , the reaction steps are simple, the thermal stability is good

Inactive Publication Date: 2014-03-26
NANJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, small molecular organophosphorus flame retardants have poor heat resistance and high volatility, and will cause some physical properties of materials to decline

Method used

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  • Method for synthesizing polymerized phenyl phosphonate by performing solid-liquid two-phase reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Dissolve 170g of NaOH in 4L of water to prepare NaOH solution, add 456g of bisphenol A into the reaction vessel, slowly pour all the NaOH solution into the reaction vessel, under the protection of nitrogen, stir at room temperature until completely dissolved, and form a salt . The water was distilled off under reduced pressure, and after vacuum drying, 530 g of bisphenol A disodium salt was obtained as a white solid.

Embodiment 2

[0030] Dissolve 170 g of NaOH in 4L of water to prepare a NaOH solution, add 500 g of bisphenol S into the reaction vessel, slowly pour all the NaOH solution into the reaction vessel, and stir at room temperature until completely dissolved under nitrogen protection to form a Salt. Water was distilled off under reduced pressure, and 560 g of bisphenol S disodium salt was obtained after vacuum drying.

Embodiment 3

[0032] Put 500g of bisphenol A disodium salt into the reaction vessel, weigh 70g of tetrahexylammonium chloride and put it into the reaction vessel, weigh 360g of phenylphosphonic acid dichloride and dissolve it in 12L of dichloromethane. The dichloromethane solution of acid dichloride was poured into the reaction vessel, and the temperature was raised to reflux for 2 h. The reaction mixture was washed with water for 3-4 times, the organic phase was separated, and the organic phase was concentrated to about 1.2 L, then 25 L of petroleum ether was poured into the organic phase, left to stand, the liquid was decanted, and the product was precipitated at the bottom. The product at the bottom was dried at 70°C, agglomerated into a solid after cooling, and pulverized.

[0033] The product was a white waxy solid with a mass of 601 g and a yield of 93.2%.

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Abstract

The invention discloses a method for synthesizing polymerized phenyl phosphonate by performing a solid-liquid two-phase reaction. The method is characterized by comprising the following steps of: performing a solid-liquid two-phase reaction on a disodium salt of dihydric phenol and phenylphosphonyl dichloride serving as raw materials in dichloromethane serving as a solvent under the action of a phase transfer catalyst; and performing a condensation polymerization reaction on the disodium salt of dihydric phenol and phenylphosphonyl dichloride to obtain a polymerized phenyl phosphonate flame retardant. The synthesis method disclosed by the invention has the advantages of simple process, no need of high-temperature reaction, no release of hydrogen chloride gas and simple post-treatment process. The solid phenyl phosphonate flame retardant has the advantages of high thermal stability, high decomposing temperature and wide applications in the material fields of epoxy resin, polyester, polyurethane, polyolefin, nylon and the like.

Description

technical field [0001] The invention relates to a preparation method of a phosphonate flame retardant, in particular to a method for synthesizing polymeric phenylphosphonate by solid-liquid two-phase reaction. Background technique [0002] Flame retardant is a functional additive that imparts flame retardancy to flammable materials (including plastics, rubber, fibers, etc.), which can delay combustion and suppress smoke. With the increasing awareness of safety and environmental protection, people have higher and higher requirements for the flame retardant properties of materials. Chlorine-free, low-smoke, and low-toxicity are the goals pursued by the continuous development of flame retardants. Organophosphorus flame retardants are in line with this development trend. However, small molecular organophosphorus flame retardants have poor heat resistance and high volatility, and will cause some physical properties of materials to decline. Polymeric polymer phosphonate flame re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G79/04C08L85/02
Inventor 肖亚平冯根锋王元元
Owner NANJING NORMAL UNIVERSITY
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