Preparation method of aryl silicon cyclic phosphate compound

A technology of phosphine compounds and aryl groups is applied in the field of preparation of flame retardant phenyl trisilane compounds, which can solve the problems of poor electrical performance, high price, restricted development, etc., and achieves the effect of promoting flame retardant, small mechanical properties, and preventing melting dripping effect

Active Publication Date: 2016-03-09
SUZHOU UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, traditional organophosphorus flame retardants still have disadvantages such as high polarity, easy migration, and poor electrical properties.
Silicone-based flame retardants are a new type of halogen-free flame retardants, which have the advantages of high efficiency, non-toxicity, smoke suppression, and environmental friendliness, but they have problems such as high prices, which limit their development.

Method used

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  • Preparation method of aryl silicon cyclic phosphate compound
  • Preparation method of aryl silicon cyclic phosphate compound
  • Preparation method of aryl silicon cyclic phosphate compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1 In a 200ml four-necked 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 60ml of ethylene glycol diethyl ether and 34.92g (0.18mol) of 4- Hydroxymethyl-4-ethyl-cyclic methyl phosphonate, add 10.58g (0.05mol) phenyltrichlorosilane dropwise under stirring, control the dropping temperature not to exceed 60°C, and raise the temperature to 110°C after dropping, React for 19 hours, after the hydrogen chloride is released, change it to a vacuum distillation device, and remove ethylene glycol diethyl ether (recycled) by vacuum distillation, then add 55ml of distilled water, stir to disperse the solid in water, suction filter, and rinse with water until pH = 7, drying to obtain a white solid aryl silicon cyclic phosphine compound, the product yield is 90.5%.

Embodiment 2

[0024] Example 2 In a 200ml four-necked 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 70ml xylene and 31.04g (0.16mol) 4-hydroxymethyl -4-Ethyl-cyclic methyl phosphonate, add 10.58g (0.05mol) phenyltrichlorosilane dropwise under stirring, control the dropping temperature not to exceed 60°C, raise the temperature to 100°C after dropping, react for 21h, After the hydrogen chloride is discharged, change it to a vacuum distillation device, and remove xylene by vacuum distillation (recycling), then add 70ml of distilled water, stir to disperse the solid in water, filter with suction, wash with water until pH = 7, and dry , to obtain a white solid aryl silicon cyclic phosphine compound with a product yield of 84.2%.

Embodiment 3

[0025] 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, replace the air in the bottle with nitrogen, and add 50ml of diethylene glycol dimethyl ether and 32.98g (0.17mol) 4-Hydroxymethyl-4-ethyl-cyclic methylphosphonate, add 10.58g (0.05mol) phenyltrichlorosilane dropwise under stirring, control the dropping temperature not to exceed 60°C, and raise the temperature to 150°C after dropping ℃, reacted for 13 hours, after the hydrogen chloride was released, it was changed to a vacuum distillation device, diethylene glycol dimethyl ether (recycled) was removed by vacuum distillation, and then 60ml of distilled water was added, stirred to disperse the solid in water, suction filtered, Rinse with water to pH = 7, and dry to obtain a white solid arylsilyl phosphine compound with a product yield of 86.0%.

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Abstract

The invention relates to a preparation method of an aryl silicon cyclic phosphate compound as a fire retardant. The structural formula of the compound is as shown in the specification. The preparation method comprises the following steps: replacing the air in a reactor with a hydrogen chloride absorption device with nitrogen; reacting phenyl trichlorosilane with 1-oxy-1-methyl-4-ethyl-4-hydroxymethyl-2,6-dioxa-1-phosphorinane in an organic solvent at 100-150 DEG C for 13-21h, wherein the mole ratio of the two substances is 1:3 to 1:3.8; and after the hydrogen chloride is all released, purifying the product to obtain the aryl silicon cyclic phosphate compound. The fire retardant is stable in physical and chemical performance, high in decomposition temperature, good in fire retarding effect, simple in preparation process, low in equipment investment and easy to produce in large scale, is suitable for being as a fire retardant of the materials such as polyester PBT, PET, polyurethane, nylon, epoxy resin and polyvinyl chloride, and has good application and development prospects.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant aryl silicon cyclic phosphine compound, in particular to a flame retardant phenyl tris(1-oxo-1-methyl-4-ethyl-1-phospha-2, The preparation method of 6-dioxa-cyclohexyl-<4>-methoxy)silane compound, the compound contains phosphorus and silicon dual flame retardant elements, phosphorus and silicon synergistically have higher flame retardant performance, and are suitable for use as Flame retardant for polyester PBT, PET, polyurethane, nylon, epoxy resin, polyvinyl chloride and other materials. Background technique [0002] Due to the extensive use of flammable organic synthetic polymer materials, the research and development of flame retardant materials has been promoted. Among flame retardant materials, halogenated flame retardants are the most widely used flame retardants, which have good flame retardant effect and wide application range. However, because halogen-based flame retar...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08L67/02C08K5/5435
CPCC07F9/657181C08K5/5435C08L2201/02C08L67/02
Inventor 王彦林李果布麦热姆·依比热依木
Owner SUZHOU UNIV OF SCI & TECH
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