Compound bis-spirophosphoryl nitrogen silane and preparation method thereof

A spirocyclic phosphorylazide silane and compound technology, applied in the field of compound double spirophosphorylazidesilane and its preparation, to achieve the effect of mild reaction conditions, high thermal stability, and improved thermal stability

Active Publication Date: 2014-08-06
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problems existing in the existing phosphorus-nitrogen intumescent flame retardants, the present invention provides a compound double spirophosphoryl nitrogen silane and its preparation method

Method used

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  • Compound bis-spirophosphoryl nitrogen silane and preparation method thereof
  • Compound bis-spirophosphoryl nitrogen silane and preparation method thereof
  • Compound bis-spirophosphoryl nitrogen silane and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The preparation method of compound double spirophosphoryl nitrogen silane, the steps are:

[0024] In the first step, dissolve 4.2mL (20.0mmol) hexamethyldisilazane in 10mL (20.0mmol) tetrahydrofuran at 0°C and nitrogen atmosphere, stir well and drop into 8mL (20.0mmol) n-butyl Lithium, after the dropwise addition, return to room temperature, and react for 1 hour; after the reaction, obtain a tetrahydrofuran solution of lithium hexamethyldisilazide, and set aside;

[0025] In the second step, add lithium hexamethyldisilazide tetrahydrofuran solution and 2.4g (8.0mmol) 3,9-dichloro-2,4, 8,10-tetraoxo-3,9-diphosphospirocyclo[5,5]-3,9-dioxundecane, reacted at -10°C for 6 hours, then returned to room temperature for 12 hours, filtered, The filtrate was rotary evaporated to obtain a solid primary product, which was washed three times with n-hexane and then once with anhydrous acetonitrile. After drying, 5.1 g of the compound bisspirophosphorylazidesilane was obtained, with ...

Embodiment 2

[0027] The preparation method of compound double spirophosphoryl nitrogen silane, the steps are:

[0028] The first step is to dissolve 8.4mL (40.0mmol) hexamethyldisilazane in 20mL (40.0mmol) tetrahydrofuran at 0°C and nitrogen atmosphere, stir well and drop into 16mL (40.0mmol) n-butyl Lithium, after the dropwise addition, return to room temperature, and react for 1.2h; after the reaction, obtain a tetrahydrofuran solution of lithium hexamethyldisilazide, and set aside;

[0029] In the second step, add lithium hexamethyldisilazide tetrahydrofuran solution and 5.3 g (18.0 mmol) 3,9-dichloro-2,4, 8,10-tetraoxo-3,9-diphosphospirocyclo[5,5]-3,9-dioxundecane, reacted at 0°C for 1 hour, then returned to room temperature for 12 hours, filtered, and the filtrate The solid primary product was obtained by rotary evaporation, which was washed twice with n-hexane and then once with anhydrous acetonitrile. After drying, 8.7 g of the compound bisspirophosphorylazidesilane was obtained, w...

Embodiment 3

[0031] The preparation method of compound double spirophosphoryl nitrogen silane, the steps are:

[0032] The first step is to dissolve 16.8mL (80.0mmol) hexamethyldisilazane in 40mL (80.0mmol) tetrahydrofuran at 0°C and nitrogen atmosphere, stir well and drop into 32mL (80.0mmol) n-butyl Lithium, after the dropwise addition, return to room temperature, and react for 1.5h; after the reaction, obtain a tetrahydrofuran solution of lithium hexamethyldisilazide, and set aside;

[0033] In the second step, add lithium hexamethyldisilazide tetrahydrofuran solution and 10.0 g (33.3 mmol) 3,9-dichloro-2,4, 8,10-tetraoxo-3,9-diphosphospirocyclo[5,5]-3,9-dioxundecane, reacted at -20°C for 3 hours, then returned to room temperature for 12 hours, filtered, The filtrate was rotary evaporated to obtain a solid primary product, which was washed three times with n-hexane and then once with anhydrous acetonitrile. After drying, 16.0 g of the compound bisspirophosphorylazidesilane was obtained...

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Abstract

The invention relates to a novel spirophosphoryl compound and particularly relates to a compound bis-spirophosphoryl nitrogen silane and a preparation method thereof. The preparation method comprises the following steps: S1, at a temperature of 0 DEG C and under a nitrogen atmosphere, dissolving hexamethyl bisilazane in tetrahydrofuran, uniformly stirring and dropwise adding n-butyllithium, and after dropwise adding n-butyllithium, recovering to room temperature and reacting for 1-1.5 hours; after reaction, obtaining a tetrahydrofuran solution of hexamethyl silylamino lithium for later use; S2, at a temperature of minus 20 DEG C and under a nitrogen atmosphere, adding the tetrahydrofuran solution of hexamethyl silylamino lithium and 3,9-dichloro-2,4,8,10-tetrahydro-3,9-diphosphorus spiro[5, 5]-3,9-dioxy undecane into the solvent, reacting for 1-6 hours under a condition that the temperature ranges from minus 20 DEG C to 0 DEG C, recovering to room temperature and reacting for 12 hours, filtering, spirally steaming the filtrate to obtain a solid initial product, washing respectively by normal hexane and anhydrous acetonitrile, and drying to obtain the compound bis-spirophosphoryl nitrogen silane.

Description

technical field [0001] The invention relates to a novel spirocyclic phosphoryl compound, in particular to a double spirophosphorylazide silane compound and a preparation method thereof. Background technique [0002] Spirocyclic phosphoryl compounds have a cage structure containing phosphorus and oxygen heteroatoms. This type of structure has good thermal stability and can generate a large amount of carbon and acid during combustion. It is an excellent carbon source and acid sources. Using spirophosphoryl chloride as a monomer, other structures containing flame retardant elements can be introduced. At present, it is more common to introduce a nitrogen-rich structure, organically combine carbon sources, acid sources and gas sources in a unified molecule, and obtain a series of phosphorus-nitrogen intumescent flame retardants. The introduction of nitrogen elements can give full play to the synergistic effect of phosphorus and nitrogen elements, improve the thermal stability o...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5445
Inventor 刘亚青梁文俊赵培华赵贵哲
Owner ZHONGBEI UNIV
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