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Polymer type phosphorous flame retardant containing DOPO and preparation method thereof

A polymer and flame retardant technology, applied in the field of polymer-type phosphorus-containing flame retardants and their preparation, can solve the problems of poor polymer matrix compatibility, leaching, and large environmental pollution, and achieve good expansion into Carbon, good flame retardant effect, high phosphorus content

Active Publication Date: 2010-11-10
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. CN1563152A proposes a method for preparing a polymer-type phosphorus-containing flame retardant, which uses DOPO-modified hydroquinone or hydronaphthalenediol, phenyl or naphthyl-substituted dichloro (bromo) oxygen Phosphorus is used as a reaction matrix to obtain a phosphorus-containing polymer flame retardant, but a catalyst must be used in the preparation process of the flame retardant, and a precipitant 5-10 times the amount of solvent is used in the separation process, which causes great pollution to the environment
This phosphorus-containing flame retardant is a small molecule phosphorus-containing compound, which has poor compatibility with the polymer matrix and has leaching problems

Method used

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  • Polymer type phosphorous flame retardant containing DOPO and preparation method thereof
  • Polymer type phosphorous flame retardant containing DOPO and preparation method thereof
  • Polymer type phosphorous flame retardant containing DOPO and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Add 29.7g of pentaerythritol diphosphate diphosphoryl chloride, 250ml of anhydrous acetonitrile and 37.2g of 9,10-dihydro-9-oxa-10-phosphorus in a 500ml three-neck flask equipped with a stirrer, nitrogen inlet and condenser Heterophenanthrene-10-oxide-p-hydroxybenzyl alcohol (DOPO-HB), heated to 80 °C under the protection of nitrogen atmosphere, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure to obtain White solid product in 90% yield.

[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. exist 1 In the HNMR spectrogram, the alcoholic hydroxyl group at 6.2 ppm and the phenolic hydroxyl group at 9.35 ppm of the product disappeared. It can be seen that the prod...

Embodiment 2

[0034] Add 29.7g of pentaerythritol diphosphate diphosphoryl chloride, 250ml of anhydrous acetonitrile and 62.2g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Oxide-tere-phenylenedimethanol (2DOPO-TDCA), heated to 80°C under the protection of nitrogen atmosphere, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure to obtain a white solid product, product The rate reached 86%.

[0035] 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. exist 1 In the HNMR spectrogram, the aldehyde absorption peak of the product at 10.0 ppm disappeared. It can be seen that the product is a polymer-type phosphorus-containing flame retardant containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene...

Embodiment 3

[0038] Add 29.7g of pentaerythritol diphosphate diphosphoryl chloride, 150ml of anhydrous acetonitrile and 69.1g of 9,10-dihydro-9-oxa-10-phosphorus in a 500ml three-necked flask equipped with a stirrer, nitrogen inlet and condenser Heterophenanthrene-10-oxide-dihydroxydiphenylmethane (2DOPO-PhOH), heated to 80°C under the protection of nitrogen atmosphere, reacted under continuous stirring until no HCl gas was released, cooled to room temperature, and removed the solvent under reduced pressure, The product was obtained as a white solid in 83% yield.

[0039] Infrared analysis is carried out to the obtained product, in pentaerythritol diphosphate diphosphoryl chloride, 583-541cm -1The 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 is a polymer-type phosphorus-containing flame retardant containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide.

[004...

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Abstract

The invention discloses a polymer type phosphorous flame retardant containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and a preparation method thereof. The invention is characterized in that: according to a reaction mole ratio, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-modified aryl dihydric phenol or 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-modified aryl dihydric alcohol and substituted phosphate dichloride are heated to 75DEG C to 80DEG C in anhydrous acetonitrile under inert atmosphere, stirred to react until halogen-free hydrogen gas is released, cooled to the room temperature and depressurized to remove solvent; the limited oxygen index of the obtained product in flame-retardant epoxy resin is greatly increased, and the vertical burning scale reaches V-0; and the flame retardant overcomes the defects of the conventional micromolecular phosphorous flame retardant, i.e. low thermal decomposition temperature, poor compatibility with polymeric matrix and easy migration, contains higher phosphorus content than the conventional polymer type phosphorous flame retardant, and has good intumescence and char formation property and good flame-retarding effect.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-containing flame retardants, in particular to polymer-type phosphorus-containing flame retardants containing 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO for short) and its preparation method. Background technique [0002] Polymer materials have been widely used in many technical fields such as aerospace, electronic information, household appliances, and automobile industry due to their abundant sources of raw materials, convenient manufacturing, various varieties, and excellent comprehensive performance. However, most of them are flammable materials, which are easy to cause fire and pose a great threat to life and property safety. 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 ...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L63/00C08L85/02
Inventor 胡源王鑫宋磊邢伟义
Owner UNIV OF SCI & TECH OF CHINA
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