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Preparation method and application of reactive type halogen-free flame-retardant polyether glycol

A flame-retardant polyether, reactive technology, applied in the field of organic synthesis, can solve the problems of containing a large amount of halogen, low functionality, high price, etc., and achieve the effects of good stability, good compatibility and moderate viscosity

Inactive Publication Date: 2016-07-27
JIANGYIN POLYTECHNIC COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the above-mentioned shortcomings, provide a preparation method and application of a reactive halogen-free flame-retardant polyether polyol, and solve the problems of high price, excessive viscosity, low functionality and Problems with high levels of halogens

Method used

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  • Preparation method and application of reactive type halogen-free flame-retardant polyether glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 271 g of tetrakis hydroxymethyl phosphorus sulfate aqueous solution (containing 203 g of tetrakis hydroxymethyl phosphorus sulfate), add 56 g of potassium hydroxide into a 1L three-necked flask equipped with mechanical stirring, thermometer and condenser tube, cool to 0°C and maintain this temperature Stir for 5 hours.

[0023] The product obtained in the first step reaction was distilled off under reduced pressure to remove the solvent water, and then 62g of ethanol was added at room temperature to dissolve the product, and then sent to a centrifuge to remove solid by-products, and then heated to 80°C and stirred for 3 hours. The ethanol was distilled off under reduced pressure to obtain the product trihydroxymethylphosphine oxide, and the reaction yield was 96%.

[0024] Weigh 124g of the product obtained in the third step reaction, add 0.62g of triethylamine into a pressure reactor, and start feeding propylene oxide when the temperature rises to about 80°C. Dur...

Embodiment 2

[0026] Weigh 253g of tetrakishydroxymethylphosphorus chloride aqueous solution (containing 190g of tetrakishydroxymethylphosphorus chloride), add 148g of calcium hydroxide into a 1L three-necked flask equipped with mechanical stirring, thermometer and condenser, and cool to -10°C Stirring was maintained at this temperature for 3 hours.

[0027] The product obtained in the first step reaction was distilled off under reduced pressure to remove the solvent water, and then 41g of methanol was added at room temperature to dissolve the product, and then sent to a centrifuge to remove solid by-products, and then heated to 70°C and stirred for 2 hours. After the reaction was completed, Methanol was distilled off under reduced pressure to obtain the product trihydroxymethylphosphine oxide, and the reaction yield was 95%.

[0028] Weigh 130g of the product obtained in the third step reaction, add 1g of potassium hydroxide into a pressure reactor, and start feeding propylene oxide when t...

Embodiment 3

[0030] Weigh 314 g of tetrakis hydroxymethyl phosphorus bromide aqueous solution (containing 235 g of tetrakis hydroxymethyl phosphorus bromide), add 200 g of sodium hydroxide into a 1L three-necked flask equipped with mechanical stirring, thermometer and condenser tube, and cool to -20°C Stirring was maintained at this temperature for 8 hours.

[0031] The product obtained in the first step reaction was distilled off under reduced pressure to remove the solvent water, and then 31g of acetone was added at room temperature to dissolve the product, and then sent to a centrifuge to remove solid by-products, and then heated to 50°C and stirred for 5 hours. The acetone was distilled off under reduced pressure to obtain the product trihydroxymethylphosphine oxide, and the reaction yield was 95%.

[0032]Weigh 132g of the product obtained in the third step reaction, add 0.8g of sodium hydroxide into a pressure reactor, and start feeding ethylene oxide when the temperature rises to ab...

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Abstract

The invention relates to a preparation method of reactive type halogen-free flame-retardant polyether glycol and belongs to the field of organic synthesis.The preparation method comprises the steps that tetramethylol phosphide is subjected to a formaldehyde removal reaction under the action of a catalyst, and then an oxidation reaction is conducted in certain solvent and at a certain temperature, so that trisphosphine oxide is prepared ; after purification is conducted, a product and epoxypropane / oxirane are subjected to an addition reaction in a certain pressure environment and a catalyst condition, so that a product, namely reactive type halogen-free flame-retardant polyether glycol, is obtained.By means of the method, raw materials are low in price and easy to obtain, the reactions are simple and controllable, the yield reaches 95% or above, the obtained reactive type halogen-free flame-retardant polyether glycol is medium in viscosity and good in compatibility with foaming agents and other auxiliary agents, a combined material compounded with the reactive type halogen-free flame-retardant polyether glycol is uniform, transparent, good in fluidity and good in stability, and certain industrial prospect is achieved.

Description

technical field [0001] The invention relates to a preparation method and application of a reactive halogen-free flame-retardant polyether polyol which can be used for flame-retardant polyurethane rigid foam materials, and belongs to the field of organic synthesis. Background technique [0002] Rigid polyurethane foam has excellent thermal insulation properties, light weight, good dimensional stability, and easy molding. It is usually used as thermal insulation materials in building insulation, refrigeration, transportation, and chemical industries. However, its flammability is the biggest problem limiting the application range of rigid polyurethane foam. At present, the main way to solve this problem is to add flame retardants in the material preparation process. Flame retardants suitable for rigid polyurethane foam can be divided into two categories: additive type and reactive type. Among them, the additive flame retardant is a compound containing certain flame retardant ...

Claims

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Application Information

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IPC IPC(8): C08G65/28C08G18/50C08G18/42
CPCC08G18/4018C08G18/5078C08G65/2639C08G2110/0025C08G2110/005
Inventor 徐娜胡娜尤勇军陆蕾蕾宋功品陆晓燕
Owner JIANGYIN POLYTECHNIC COLLEGE
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