Technique for preparing hexabromocyclophosphazene trimer

A technology of hexabromocyclotripolyphosphazene and a new process is applied in the field of chemical synthesis, can solve the problems of low cost, high cost, low yield and the like, and achieves the effects of mild reaction process conditions, high success rate and high yield

Inactive Publication Date: 2008-09-17
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has low cost, but compared with phosphorus tribromide, it is difficult for solid red phosphorus to form phosphorus pentabromide with liquid bromine, resulting in long reaction time and low yield
It is precisely because of the low yield of hexabromocyclotrimeric phosphazene that its cost is high and it is not suitable for industrial production, which limits the application of phosphazene compounds

Method used

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  • Technique for preparing hexabromocyclophosphazene trimer
  • Technique for preparing hexabromocyclophosphazene trimer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 15g dry ammonium bromide, 10ml phosphorus tribromide, 200ml chlorobenzene and 6.0ml, 0.5g CaCl 2 , a composite catalyst composed of 0.5g ZnO. Heating to reflux with stirring to boiling, quickly drop 3.0ml of liquid Br into the three-necked flask 2 , Control the temperature of the reaction system at 130°C to 140°C. After reacting for 1 hour, add 1.0 g of dry ammonium bromide and continue to slowly add 3.0 ml of liquid Br 2 . After 1 hour, 1.0 g of dry ammonium bromide was added, and the reaction was continued for 4 hours before heating was stopped. The unreacted ammonium bromide was filtered out while hot, and the filtrate was distilled under reduced pressure until a small amount of crystals were precipitated. The distillation residue was rapidly cooled, and white crystals precipitated. The obtained white crystals were dissolved in toluene and recrystallized to obtain a white crystalline hexabromocyclotrimeric phosphazene product with a yield of 51%.

Embodiment 2

[0022] Add 15g of dry ammonium bromide, 10ml of phosphorus tribromide, 200ml of chlorobenzene, and 6.0ml of pyridine, 0.5g of CuCl 2 and 0.5g CaO composite catalyst. Heating to reflux with stirring to boiling, quickly drop 3.0ml of liquid Br into the three-necked flask 2 , Control the temperature of the reaction system at 130°C to 140°C. After reacting for 1 hour, then add 1.0 g of dry ammonium bromide, continue to slowly add 3.0 ml of liquid Br2. After 1 hour, add 1.0 g of dry ammonium bromide, and continue the reaction for 4 hours before stopping heating. The unreacted ammonium bromide was filtered out while hot, and the filtrate was distilled under reduced pressure until a small amount of crystals were precipitated. The distillation residue was rapidly cooled, and white crystals precipitated. The obtained white crystals were dissolved in toluene and recrystallized to obtain a white crystalline hexabromocyclotrimeric phosphazene product with a yield of 43%.

Embodiment 3

[0024] Add 15g dry ammonium bromide, 10ml phosphorus tribromide, 200ml chlorobenzene and 6.0ml 4-picoline, 0.5g CoCl 2 , 0.5g NiCl 2 composed of composite catalysts. Heating to reflux with stirring to boiling, quickly drop 3.0ml of liquid Br into the three-necked flask 2 , Control the temperature of the reaction system at 130°C to 140°C. After reacting for 1 hour, add 1.0 g of dry ammonium bromide and continue to slowly add 3.0 ml of liquid Br 2 . After 1 hour, 1.0 g of dry ammonium bromide was added, and the reaction was continued for 4 hours before heating was stopped. The unreacted ammonium bromide was filtered out while hot, and the filtrate was distilled under reduced pressure until a small amount of crystals were precipitated. The distillation residue was rapidly cooled, and white crystals precipitated. The resulting white crystals were dissolved in toluene and recrystallized to obtain a white crystalline hexabromocyclotrimeric phosphazene product with a yield of 3...

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Abstract

The invention discloses a novel process for preparing hexabromocyclotriphosphazene. The process is characterized in charging step by step and including allowing ammonium bromide, phosphorus tribromide and liquid bromine to react in chlorobenzene in the presence of high efficiency polybasic composite catalyst, and purifying the product through freeze separation. The product has a purity of greater than 98% and a yield of about 50%. Compared with the conventional method, the process has the advantages of short reaction time and high product yield.

Description

technical field [0001] The invention relates to a new process for preparing fine chemical intermediates, in particular to a new process for preparing hexabromocyclotrimeric phosphazene, which belongs to the field of chemical synthesis. Background technique [0002] Phosphazene compounds are a class of linear or cyclic compounds whose skeletons are alternately arranged with phosphorus atoms and nitrogen atoms. Cyclic phosphazene compounds are a class of polycyclic ring compounds with alternating P and N atoms as the skeleton. It is an important chemical intermediate, and its structural formula is (NPR 2 )n, n=3-9, representative compounds are hexachlorocyclotrimeric phosphazene and hexabromocyclotrimeric phosphazene. Polyphosphazene compounds mainly refer to linear low-molecular or linear high polymers whose main chain is composed of alternating P and N atoms and alternating single and double bonds. The diversification of the side groups of phosphazene compounds endows the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593
Inventor 徐建中李木子谢吉星屈红强王春征何勇武李妍
Owner HEBEI UNIVERSITY
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