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A novel macromolecular sulfur-containing organic phosphine flame retardant compound and preparation method thereof

A compound and organic phosphine technology, which is applied in the field of polyphenylthiophosphonic acid ethylene glycol ester and its preparation, can solve problems such as safety threats, and achieve the effects of good compatibility, large molecular weight, and difficult migration

Active Publication Date: 2011-12-14
SUNSHINE INFLATABLE TOYS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, while it brings convenience to the society, it also brings a series of problems that cannot be ignored. In particular, its own flammability poses a threat to people's safety, so it is urgent to develop new flame-retardant polymer materials. the urgency of

Method used

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  • A novel macromolecular sulfur-containing organic phosphine flame retardant compound and preparation method thereof
  • A novel macromolecular sulfur-containing organic phosphine flame retardant compound and preparation method thereof
  • A novel macromolecular sulfur-containing organic phosphine flame retardant compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 In a 150ml three-neck flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol, 0.2g of anhydrous zinc chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenyl phosphonothioate dichloride, dropwise the addition in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 3 hours, and then react for 7 hours under reduced pressure through the hydrogen chloride absorption device, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 76%, its melting point is 175°C, and its decomposition temperature is 288°C.

Embodiment 2

[0026] Example 2 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol and 0.2g of anhydrous aluminum chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenyl phosphonothioate dichloride, drop it in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 4 hours, and then react for 6 hours under reduced pressure through the hydrogen chloride absorption device, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 71%, its melting point is 175°C, and its decomposition temperature is 288°C.

Embodiment 3

[0027] Example 3 In a 150ml three-necked flask equipped with a stirrer, a thermometer, and a reflux condenser, add 0.35mol (21.72g) of ethylene glycol, 0.2g of anhydrous calcium chloride, and raise the temperature to 45°C under nitrogen protection to start dripping Add 0.35mol (73.87g) of phenylphosphonothioate dichloride, dropwise the addition in 2 hours, control the reaction temperature at 120°C, react at normal pressure for 5 hours, then pass the hydrogen chloride absorbing device to react under reduced pressure for 5 hours, and then transfer the reaction product to a 250ml three-port Add 100ml of N,N-dimethylformamide to the flask, heat to 100°C and keep stirring for 1 hour, cool to 25°C to completely precipitate the solid product, filter, wash with methanol, and dry to obtain white powdery solid polyphenylsulfide Ethylene glycol phosphonate. Its yield is 70%, its melting point is 175°C, and its decomposition temperature is 288°C.

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Abstract

The invention relates to a new macromolecular sulfur-containing organophosphorus flame-retardant compound of the following formula and a preparation method thereof, wherein, n is larger than 1. The preparation method comprises the following steps: in the presence of nitrogen, carrying out heating reaction on equimolar phenylphosphonothioic dichloride and glycol in the presence of catalysts for a period of time, then carrying out purification and drying on the reactant to obtain polyphenyl thiophosphate gylcol ester. The prepared compound has high flam resistance, stable physical and chemical characteristics, and good intermiscibility with high polymer materials, and is suitable for the flame-resistant treatment of polyurethane and other materials. The method has the advantage of simple process and is easy to realize industrial production.

Description

technical field [0001] The invention relates to a novel macromolecule sulfur-containing organic phosphine flame retardant and a preparation method thereof, in particular to a polyphenylethylene glycol thiophosphonate and a preparation method thereof. Background technique [0002] The development and application of polymer materials is a symbol of the development of human science and technology. However, while it brings convenience to the society, it also brings a series of problems that cannot be ignored. In particular, its own flammability poses a threat to people's safety, so it is urgent to develop new flame-retardant polymer materials. of urgent need. At present, flame retardants have become the second largest additives after plasticizers in polymer material processing aids. The most widely used flame retardants are halogenated flame retardants. However, due to the enhancement of people's awareness of environmental protection, their use is limited. At present, the most...

Claims

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Application Information

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IPC IPC(8): C08G79/04C08L75/04C08L67/00C08L63/00C08L85/02
Inventor 王彦林张艳丽杨小琴
Owner SUNSHINE INFLATABLE TOYS CO LTD