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Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof

A phosphorus flame retardant, polymeric technology, applied in the field of polymeric phosphorus-containing flame retardants and its preparation, can solve the problems of large environmental pollution, leaching, poor compatibility of polymer matrix, etc., and achieve good flame retardant effect , Overcoming the effect of low thermal decomposition temperature and good expansion into charcoal

Active Publication Date: 2009-12-30
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chinese Patent Application Publication No. CN1910263A introduces a method for preparing a phosphorus-containing flame retardant, which involves reacting the organic phosphorus compound DOPO with an unsaturated acid or its anhydride in alkylene glycol, but the phosphorus-containing flame retardant prepared by this method The agent is some small molecule phosphorus-containing compound, which has poor compatibility with the polymer matrix and has leaching problems.
A catalyst is used in the preparation process of the flame retardant, and a large amount of precipitant is used in the separation process, which causes great pollution to the environment.

Method used

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  • Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof
  • Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof
  • Polymeric phosphorus-containing flame retardant with DOPO as lateral group and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 29.7g (0.10mol) of pentaerythritol diphosphate diphosphoryl chloride, 150ml of anhydrous acetonitrile and 32.4g (0.10mol) of 9,10-dihydro -9-oxa-10-phosphaphenanthrene-10-oxide-hydroquinone, heat up to 80°C, react under continuous stirring until no HCl gas is released, cool to room temperature, remove the solvent under reduced pressure, and obtain pink Colored solid product. The yield is 95%, and the melting point is 220°C.

[0026] Infrared analysis is carried out to the obtained product, in pentaerythritol diphosphate diphosphoryl chloride, 583-541cm -1 The characteristic peak of P-Cl bond disappears at 929, 1189cm -1 P-O-Ph characteristic peak at 1442cm -1 P-Ph characteristic peak appears. It can be seen that the product of this example is a polymeric phosphorus-containing flame retardant with side groups of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

[0027] Take 6.6 grams of the polymeric phosphorus-containing flame retardant whose side group is ...

Embodiment 2

[0030] Add 29.7g (0.10mol) of pentaerythritol diphosphate diphosphoryl chloride, 150ml of anhydrous acetonitrile and 39.8g (0.10mol) of 9,10-dihydro -9-Oxa-10-phosphaphenanthrene-10-oxide-p-naphthalenediol, heated to 80°C, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure to obtain a pink solid product. The yield was 92%, and the melting point was 235°C.

[0031] Infrared analysis is carried out to the obtained product, in pentaerythritol diphosphate diphosphoryl chloride, 583-541cm -1 The characteristic peak of P-Cl bond disappears at 929, 1189cm -1 P-O-Ph characteristic peak at 1442cm -1 P-Ph characteristic peak appears. It can be seen that the product of this example is a polymeric phosphorus-containing flame retardant with side groups of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

[0032] Take 6.6 grams of the polymeric phosphorus-containing flame retardant prepared in ...

Embodiment 3

[0035] Add 29.7g (0.10mol) of pentaerythritol diphosphate diphosphoryl chloride, 150ml of anhydrous acetonitrile and 39.8g (0.10mol) of 9,10-dihydro -9-Oxa-10-phosphaphenanthrene-10-oxide-bisphenol A, heated to 80°C, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure to obtain a red solid product. The yield was 85%, and the melting point was 240°C.

[0036] Infrared analysis is carried out to the obtained product, in pentaerythritol diphosphate diphosphoryl chloride, 583-541cm -1 The characteristic peak of P-Cl bond disappears at 929, 1189cm -1 P-O-Ph characteristic peak at 1442cm -1 P-Ph characteristic peak appears. It can be seen that the product obtained in this example is a polymeric phosphorus-containing flame retardant with side groups of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

[0037] Get 6.6 grams of the polymeric phosphorus-containing flame retardant whose side g...

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Abstract

The invention discloses a polymeric phosphorus-containing flame retardant with 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide as a lateral group and a preparation method thereof. The preparation method is characterized by comprising the following steps: placing aromatic dihydric phenol and pentaerythritol diphosphate diphosphoryl chloride (or bromine) which are modified by the 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in an anhydrous acetonitrile solvent based on reaction mol ratio, heating the obtained mixture to 80 DEG C in an inert atmosphere, agitating and reacting until no halogen hydride is released, cooling the obtained mixture to the room temperature, and depressurizing the mixture to remove the solvent. The obtained product has high phosphorus content, very good expansibility and char formation, and good flame retardation effect. When flame retardation is performed on epoxy resin, the limiting oxygen index of the obtained product is greatly improved and the vertical burning scale reaches V-0 level; and the polymeric phosphorus-containing flame retardant has the advantage of overcoming the disadvantages of low thermal decomposition temperature, poor compatibility with polymer matrix and easy migration in the existing micromolecular phosphorus flame retardants. The preparation method has the advantages of being simple and feasible, using no catalyst and simple post-treatment process.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame retardants, in particular to a polymeric phosphorus-containing flame retardant whose side group is 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short) and its preparation method. Background technique [0002] At present, products made of polymers such as epoxy resins, unsaturated resins and polyamides have been widely used in various aspects of life and production, but most of them are flammable materials that are easy to cause fires and are harmful to life and property. pose a great threat. Therefore, the flame retardancy of polymer materials has become a hot issue to be solved urgently. At present, it is widely used to add flame retardants to various polymers to improve their flame retardant properties. Phosphorus-based flame retardants have been extensively studied by many scholars at home and abroad for their advantages of high efficiency, low toxicity, a...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08G79/04C09K21/14C09K21/12
Inventor 胡源王鑫宋磊邢伟义
Owner UNIV OF SCI & TECH OF CHINA
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