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Preparation method of flame retardant organosilicon cyclic phosphine compound

A technology of phosphine compound and organosilicon, which is applied in the field of preparation of flame retardant alkyl trisilane compound, can solve the problems of limited application range, and achieve the effects of easy large-scale production, prevention of melt dripping, and high decomposition temperature

Active Publication Date: 2018-02-02
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, a single silicone flame retardant is only effective for the flame retardancy of some high polymers, and its application is not wide

Method used

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  • Preparation method of flame retardant organosilicon cyclic phosphine compound
  • Preparation method of flame retardant organosilicon cyclic phosphine compound
  • Preparation method of flame retardant organosilicon cyclic phosphine compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Example 1 In a 200ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device, replace the air in the bottle with nitrogen, and add 45ml of dioxane and 32.01g (0.165mol) of 4-hydroxyl Methyl-4-ethyl-cyclic methylphosphonate, add 7.47g (0.05mol) methyltrichlorosilane dropwise under stirring, control the dropwise addition temperature not to exceed 60°C, and raise the temperature to 80°C after dropping, react After 18 hours, after the hydrogen chloride was released, it was changed to a vacuum distillation device, and the dioxane (recycled) was removed by vacuum distillation, and then 35ml of distilled water was added, stirred to disperse the solid in water, suction filtered, and rinsed with water until pH = 7. Dry to obtain white solid methyl tris(1-oxo-1-methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl--methoxy base) silane, product yield 95.4%, its melting point: 75°C±2°C, decomposition temperature:...

Embodiment 2

[0036] Example 2 In a 200ml four-neck flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device, replace the air in the bottle with nitrogen, and add 65ml xylene and 29.1g (0.15mol) 4-hydroxymethyl -4-Ethyl-cyclic methylphosphonate, add 7.47g (0.05mol) methyltrichlorosilane dropwise under stirring, control the dropping temperature not to exceed 60°C, raise the temperature to 100°C after dropping, and react for 15h, After the hydrogen chloride is discharged, change it to a vacuum distillation device, and remove xylene by vacuum distillation (recycling), then add 40ml of distilled water, stir to disperse the solid in water, filter with suction, wash with water until pH = 7, and dry , to obtain white solid methyl tris(1-oxo-1-methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl--methoxy)silane, The product yield is 80.7%, its melting point: 75°C±2°C, decomposition temperature: 250°C±5°C.

Embodiment 3

[0037] Example 3 In a 200ml four-necked flask equipped with a stirrer, a thermometer, a high-efficiency reflux condenser and a hydrogen chloride absorption device, the air in the bottle was replaced with nitrogen, and 40ml of toluene and 30.07g (0.155mol) of 4-hydroxymethyl- 4-Ethyl-cyclic methylphosphonate, add 7.47g (0.05mol) methyltrichlorosilane dropwise under stirring, control the dropping temperature not to exceed 60°C, raise the temperature to 110°C after dropping, react for 13h, wait After the hydrogen chloride is released, change it to a vacuum distillation device, and remove the toluene (recycled) by vacuum distillation, then add 45ml of distilled water, stir to make the solid disperse in water, filter with suction, rinse with water until pH=7, and dry to obtain White solid methyltris(1-oxo-1-methyl-4-ethyl-1-phospha-2,6-dioxa-cyclohexyl--methoxy)silane, the product was The yield is 83.8%, its melting point: 75℃±2℃, decomposition temperature: 250±5℃.

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Abstract

The invention relates to a method for preparing a flame retardant organosilicon cyclic phosphine compound. The structure of the compound is shown in the following formula: in the formula, R=methyl, ethyl, propyl or butyl. The preparation method is: replace the air in the reactor with hydrogen chloride absorption device with nitrogen, alkyl trichlorosilane and 1-oxygen-1-methyl-4-ethyl-4-hydroxymethyl-2, 6- Dioxa-1-phosphorinane is reacted in an organic solvent with a molar ratio of 1:3-1:3.5, reacted at 80-150°C for 10-18h, and after the hydrogen chloride is released, it is purified to obtain Organosilicon phosphine compounds. The product of the present invention has high flame retardant efficiency, and also has the effect of charring and anti-dripping, and is suitable for use as a flame retardant for polyester PBT, PET, PS, PP, PC, ABS and other materials; and the production process is simple, the equipment investment is small, and it is easy to use. Realize industrialized production.

Description

technical field [0001] The invention relates to a method for preparing a flame retardant organosilicon cyclic phosphine compound, in particular to a flame retardant alkyl tris(1-oxo-1-methyl-4-ethyl-1-phospha-2,6 - Process for the preparation of dioxa-cyclohexyl-<4>-methoxy)silane compounds. The compound contains dual flame retardant elements of phosphorus and silicon. Phosphorus and silicon synergistically have higher flame retardant performance, and are suitable for use as flame retardants for polyester PBT, PET, PS, PP, PC, ABS and other materials. Background technique [0002] Silicone flame retardant is a new generation of halogen-free carbon-forming flame retardant that is highly efficient, eco-friendly, anti-melt and smoke-suppressing. It has excellent flame retardant, mechanical properties, and processing properties. Combustion has shown great potential for development. Although organosilicon-based flame retardants started relatively late, they have developed...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6574C08K5/5435
Inventor 王彦林李果
Owner SUZHOU UNIV OF SCI & TECH
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