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Preparation method and application of cyclotriphosphazene containing silicon functional groups

A technology of cyclotriphosphazene and hexachlorocyclotriphosphazene is applied in the field of flame retardant, which can solve the problems of low yield and the like, and achieve the effects of high yield, high elongation at break and high oxygen index

Active Publication Date: 2011-11-23
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to propose a preparation method and application of a silicon-containing functional group cyclotriphosphazene in order to solve the problem of low yield of the above-mentioned substances synthesized in the prior art

Method used

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  • Preparation method and application of cyclotriphosphazene containing silicon functional groups
  • Preparation method and application of cyclotriphosphazene containing silicon functional groups

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Experimental program
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Effect test

Embodiment 1

[0023] 1) Add 14.61g of aminopropyltriethoxysilane and 7.28g of triethylamine into 20ml of tetrahydrofuran solvent, stir and mix evenly, pass in argon, and slowly heat to 60°C;

[0024] 2) 3.48g of hexachlorocyclotriphosphazene was dissolved in 10ml of tetrahydrofuran solvent, magnetically stirred to make it fully dissolved, and then added dropwise to the solution in step 1), a white precipitate was gradually formed, and the dropping time was 30min, at 67 The reaction was carried out at ℃ for 10 hours; after the reaction, the obtained product was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was rotated in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group cyclotriethylamine hydrochloride. Phosphazene is a light yellow-green liquid with a yield of 90.4%.

[0025] Spectral data for phosphazene compounds containing organosilicon groups are:

[0026] FT-IR (cm -1 ): 32...

Embodiment 2

[0030] 1) Add 15.49g of aminopropyltriethoxysilane and 7.28g of triethylamine into 20ml of tetrahydrofuran solvent, stir and mix evenly, pass in argon, and slowly heat to 60°C;

[0031] 2) 3.47g of hexachlorocyclotriphosphazene was dissolved in 10ml of tetrahydrofuran solvent, magnetically stirred to make it fully dissolved, and then added dropwise to the solution in step 1), a white precipitate was gradually formed, and the time for adding was 30min. The reaction was carried out at ℃ for 10 hours; after the reaction, the obtained product was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was rotated in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group cyclotriethylamine hydrochloride. Phosphazene is a light yellow-green liquid with a yield of 93.5%.

[0032] Compound the above-mentioned 6g of silicon-containing functional group cyclotriphosphazene, 24g of ammonium po...

Embodiment 3

[0035] 1) Add 14.60g of aminopropyltriethoxysilane and 8.11g of triethylamine into 20ml of tetrahydrofuran solvent, stir and mix evenly, pass in argon, and slowly heat to 60°C;

[0036] 2) 3.48g of hexachlorocyclotriphosphazene was dissolved in 10ml of tetrahydrofuran solvent, magnetically stirred to make it fully dissolved, and then added dropwise to the solution in step 1), a white precipitate was gradually formed, and the dropping time was 30min, at 67 The reaction was carried out at ℃ for 10 hours; after the reaction, the obtained product was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was rotated in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group cyclotriethylamine hydrochloride. Phosphazene is a light yellow-green liquid with a yield of 91.4%.

[0037] Compound the 4g of silicon-containing functional cyclotriphosphazene, 26g of ammonium polyphosphate and 70...

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Abstract

The invention relates to a preparation method and application of cyclotriphosphazene containing silicon functional groups, particularly relates to a method for preparing a compound simultaneously containing phosphor, nitrogen and silicon elements, and belongs to the technical field of flame retarding. The method comprises the following step: dissolving aminopropyltriethoxysilane, triethylamine and hexachlorocyclotriphosphazene in a tetrahydrofuran solvent, heating, reacting, filtering and drying in vacuum to prepare the cyclotriphosphazene containing silicon functional groups; and the application of the cyclotriphosphazene containing silicon functional groups comprises: compounding the cyclotriphosphazene containing silicon functional groups with ammonium polyphosphate, polypropylene and an antioxidant in a certain proportion, extruding and performing injection molding to obtain flame-retardant polypropylene containing silicon functional groups. The method has the advantages of mild reacting conditions, easiness in control, good repeatability, high yield and suitability for expanded production; and the compound serving as a synergist is added into a flame retardant polypropylene system to be used as a flexibilizer and a fire retardant of the flame retardant polypropylene system, and the prepared polypropylene has the characteristics of high oxygen index and high breaking elongation.

Description

technical field [0001] The invention relates to a preparation method and application of a silicon-containing functional group cyclotriphosphazene, in particular to a preparation method and application of a compound containing phosphorus, nitrogen and silicon elements, and belongs to the technical field of flame retardancy. Background technique [0002] Phosphorus is a recognized flame retardant element, and many of the commonly used halogen-free flame retardants are phosphorus-containing flame retardants. Hexachlorocyclotriphosphazene is a cyclic phosphazene that contains both phosphorus and nitrogen elements, and has a high phosphorus content. It itself has high thermal stability. It and its derivatives have been used in polymer materials. a wide range of applications. Aminopropyltriethoxy is a commonly used silane coupling agent in polymer processing. It is an improved additive that can combine two substances with different properties through chemical or physical action. ...

Claims

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Application Information

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IPC IPC(8): C07F9/6593C08K5/544C08L23/12C08K13/02
CPCY02P20/52
Inventor 李定华何兰岚杨荣杰
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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