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Reactive intumescent flame retardant for polyurethane and synthesis method of reactive intumescent flame retardant

An intumescent flame retardant and a synthesis method technology, applied in the field of flame retardants and new intumescent flame retardants, can solve the problems of poor flame retardant effect, large amount of use, low content of phosphorus and nitrogen components, etc., and achieve easy control. , The effect of good carbon formation and high yield

Inactive Publication Date: 2012-07-18
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the content of phosphorus and nitrogen in the flame retardant is low, and the flame retardant effect is not good if it is used in a large amount.

Method used

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  • Reactive intumescent flame retardant for polyurethane and synthesis method of reactive intumescent flame retardant
  • Reactive intumescent flame retardant for polyurethane and synthesis method of reactive intumescent flame retardant
  • Reactive intumescent flame retardant for polyurethane and synthesis method of reactive intumescent flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The synthetic method of reactive expansion flame retardant for polyurethane comprises the following steps:

[0029] (1) Add 10.0 g of chlorinated spirocyclic phosphate and 50 mL of deionized water into a 250 mL reactor equipped with a stirring device and a cooling device, and stir vigorously for 5 minutes to make the chlorinated spirocyclic phosphate Evenly dispersed in water;

[0030] (2) Weigh 9.0 g of diethanolamine and dissolve it in 20 mL of deionized water, and add the aqueous solution of diethanolamine dropwise to the suspension obtained in step (1) at 3 °C under vigorous stirring;

[0031] (3) Measure 9.6 mL of triethylamine dropwise into the reaction system obtained in step (2). After the dropping is complete, raise the temperature to 55°C and react for 5 hours. yellow solution;

[0032] (4) Cool the solution obtained in step (3) to room temperature, filter, and concentrate under reduced pressure at 70°C until the volume of the solution does not change to obt...

Embodiment 2

[0038](1) Add 10.0 g of chlorinated spirocyclic phosphate and 50 mL of methanol into a 250 mL reactor equipped with a stirring device and a cooling device, and stir vigorously for 3 minutes to make the chlorinated spirocyclic phosphate evenly dissolved in the demethanol dispersion;

[0039] (2) Weigh 10.7 g of diethanolamine and dissolve it in 40 mL of deionized water, and add the aqueous solution of diethanolamine dropwise to the suspension obtained in step (1) at 0 °C under vigorous stirring;

[0040] (3) Measure 9.6 mL of triethylamine dropwise into the reaction system obtained in step (2). After the dropping is complete, raise the temperature to 60°C and react for 4 hours. yellow solution;

[0041] (4) Cool the solution obtained in step (3) to room temperature, filter, and concentrate under reduced pressure at 60°C until the volume of the solution does not change to obtain a yellow viscous liquid, which is washed 5 times with dichloromethane to purify product;

[0042] ...

Embodiment 3

[0044] (1) Add 10.0 g of chlorinated spirocyclic phosphate and 50 mL of methanol into a 250 mL reactor equipped with a stirring device and a cooling device, and stir vigorously for 4 minutes to make chlorinated spirocyclic phosphate in demethanol Evenly dispersed;

[0045] (2) Weigh 10.7 g of diethanolamine and dissolve it in 30 mL of methanol, and add the methanol solution of diethanolamine dropwise to the suspension obtained in step (1) at 5 °C under vigorous stirring;

[0046] (3) Measure 9.6 mL of triethylamine dropwise into the reaction system obtained in step (2). After the dropping is complete, raise the temperature to 50°C and react for 6 hours. yellow solution;

[0047] (4) Cool the solution obtained in step (3) to room temperature, filter, and concentrate under reduced pressure at 40°C to 1 / 3 of the volume of the original solution, then heat up to 60°C and continue to concentrate under reduced pressure until the volume of the solution does not change, to obtain Yel...

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Abstract

The invention discloses a reactive intumescent flame retardant for polyurethane and a synthesis method of the reactive intumescent flame retardant, relates to a flame retardant technology, in particular to a novel intumescent flame retardant which contains an acid source, a carbon source and a gas source simultaneously and contains a hydroxyl group serving as an active group. The chemical name ofthe reactive intumescent flame retardant for polyurethane is 3,9-di{N,N-di(2-ethoxyl)-amino}-2,4,8,10-4-oxo-3,9-diphosphate spiro-3,9-dioxo-[5,5]-undecane. The structure of the reactive intumescent flame retardant is shown as a formula (I). The synthesis method comprises the following steps of: adding 3,9-di{N,N-di(2-ethoxyl)-amino}-2,4,8,10-4-oxo-3,9-diphosphate spiro-3,9-dioxo-[5,5]-undecane into water; dropwise adding diethanolameine and triethylamine at the temperature of 0-5 DEG C; reacting at the temperature of 50-60 DEG C for 4-6 hours; concentrating under reduced pressure; purifying; and performing vacuum drying to obtain the flame retardant. The flame retardant and the synthesis method of the reactive intumescent flame retardant have the advantages of integration of phosphorus, nitrogen and carbon, high phosphorus and nitrogen flame-retardant ingredients, no containing of halogen, nontoxicity, environmental friendliness, high carbon forming property, high compatibility with apolyurethane system, simple process, mild synthesis condition and suitability for industrial implementation.

Description

technical field [0001] The invention relates to flame retardant technology, in particular to a novel intumescent flame retardant containing an acid source, a carbon source and a gas source and containing an active hydroxyl group, specifically a reactive intumescent flame retardant for polyurethane and its synthesis method. Background technique [0002] Intumescent Flame Retardant (Intumescent Flame Retardant) contains phosphorus and nitrogen flame retardant elements, and also contains acid source, carbon source and gas source. After this kind of flame retardant is heated, the compound effect of phosphorus and nitrogen in the molecule occurs, and a puffy and closed carbon foam layer is formed on the surface, which can be flame retardant, oxygen barrier, smoke elimination, anti-dripping, etc., and can release non-combustible gas , Dilute the flammable gas released by polymer combustion, therefore, it has excellent flame retardant effect, low toxicity, low smoke, and less addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C07F9/6574
Inventor 刘亚青毋登辉赵培华柳学义王晓峰张美
Owner ZHONGBEI UNIV
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