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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Problems solved by technology

[0004] The purpose of the present invention is to propose a preparation method and application of a silicon-containing functional ...
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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.

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

Examples

  • Experimental program(3)

Example Embodiment

[0022] Example 1
[0023] 1) Add 14.61g of aminopropyltriethoxysilane and 7.28g of triethylamine to 20ml of tetrahydrofuran solvent, stir and mix uniformly, pass in argon, and slowly heat to 60°C;
[0024] 2) Dissolve 3.48g of hexachlorocyclotriphosphazene in 10ml of tetrahydrofuran solvent, magnetically stir to fully dissolve it, and then add it dropwise to the solution in step 1). A white precipitate is gradually formed. The dropping time is 30min. The reaction was carried out at ℃ for 10 hours; after the reaction, the product obtained was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was revolved in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group ring three Phosphononitrile is a light yellow-green liquid with a yield of 90.4%.
[0025] The spectral data of phosphazene compounds containing organosilicon groups are:
[0026] FT-IR(cm -1 ): 3235 (-NH), 1190 (P=N), 749 (P-N); 1H NMR (CDCl3, δ, ppm, TMS): 1.238 (9H, (-CH 2 CH 3 ) 3 ), 3.833 (6H, (-CH 2 CH 3 ) 3 ), 1.87 (H, -NH).
[0027] The above synthesized 8g silicon-containing functional group cyclotriphosphazene, 22g ammonium polyphosphate and 70g polypropylene are compounded, and then 0.1g 1010 antioxidant and 0.2g 168 antioxidant are added. The extrusion temperature conditions are 165℃, 170℃ , 175°C, 180°C, 175°C, 170°C, and injection molding temperature conditions of 190°C, 195°C, 200°C, 195°C, 190°C, to obtain flame-retardant polypropylene test specimens.
[0028] According to GB/T1040.2-2006, the mechanical properties are characterized by an electronic tensile testing machine, and the elongation at break is 83.36%. According to GB/T2046.2-2009, the limiting oxygen index is characterized by an oxygen index meter. The limiting oxygen index is 26.5%.

Example Embodiment

[0029] Example 2
[0030] 1) Add 15.49g of aminopropyltriethoxysilane and 7.28g of triethylamine to 20ml of tetrahydrofuran solvent, stir and mix uniformly, pass in argon, and slowly heat to 60°C;
[0031] 2) Dissolve 3.47g of hexachlorocyclotriphosphazene in 10ml of tetrahydrofuran solvent, magnetically stir to fully dissolve it, and then add it dropwise to the solution in step 1). A white precipitate is gradually formed. The dropping time is 30min. The reaction was carried out at ℃ for 10 hours; after the reaction, the product obtained was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was revolved in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group ring three Phosphononitrile is a light yellow-green liquid with a yield of 93.5%.
[0032] The above synthesized 6g silicon-containing functional group cyclotriphosphazene, 24g ammonium polyphosphate and 70g polypropylene are compounded, and then 0.1g 1010 antioxidant and 0.2g 168 antioxidant are added. The extrusion temperature conditions are 165℃, 170℃ , 175°C, 180°C, 175°C, 170°C, and injection molding temperature conditions of 190°C, 195°C, 200°C, 195°C, 190°C, to obtain flame-retardant polypropylene test specimens.
[0033] According to GB/T1040.2-2006, the mechanical properties are characterized by an electronic tensile testing machine, and the elongation at break is 84.89%. According to GB/T2046.2-2009, the limiting oxygen index is characterized by an oxygen index meter. The limiting oxygen index is 23.9%.

Example Embodiment

[0034] Example 3
[0035] 1) Add 14.60g of aminopropyltriethoxysilane and 8.11g of triethylamine to 20ml of tetrahydrofuran solvent, stir and mix uniformly, pass in argon, and slowly heat to 60°C;
[0036] 2) Dissolve 3.48g of hexachlorocyclotriphosphazene in 10ml of tetrahydrofuran solvent, magnetically stir to fully dissolve it, and then add it dropwise to the solution in step 1). A white precipitate is gradually formed. The dropping time is 30min. The reaction was carried out at ℃ for 10 hours; after the reaction, the product obtained was suction filtered to remove the white triethylamine hydrochloride, and then the filtrate was revolved in vacuum to remove the tetrahydrofuran solvent and excess triethylamine to obtain the silicon-containing functional group ring three Phosphazene is a light yellow-green liquid with a yield of 91.4%.
[0037] The above synthesized 4g silicon-containing functional group cyclotriphosphazene, 26g ammonium polyphosphate and 70g polypropylene are compounded, and then 0.1g 1010 antioxidant and 0.2g 168 antioxidant are added. The extrusion temperature conditions are 165℃, 170℃ , 175°C, 180°C, 175°C, 170°C, and injection molding temperature conditions of 190°C, 195°C, 200°C, 195°C, 190°C, to obtain flame-retardant polypropylene test specimens.
[0038] According to GB/T1040.2-2006, the mechanical properties are characterized by an electronic tensile testing machine, and the elongation at break is 80.44%. According to GB/T2046.2-2009, the limiting oxygen index is characterized by an oxygen index meter. The limiting oxygen index is 21.5%.
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