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Halogen-free reaction type flame retardant for polyurethane foam as well as preparation method and application thereof

A reactive flame retardant, polyurethane foam technology, applied in the field of halogen-free phosphorus flame retardants, can solve the problems of high cost of DOPO, restrict the application of DOPO flame retardants, etc., to improve storage stability, improve mechanical properties and thermal properties. The effect of stability and broad application prospects

Active Publication Date: 2014-04-02
徐州市洛克尔化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Researchers from various countries have conducted a lot of research on DOPO, but due to the high cost of DOPO, the application of DOPO flame retardants is limited. By adding an alcohol amine structure to DOPO molecules, the cost of flame retardants can be greatly reduced, and benzene The existence of the ring enhances thermal stability and flame retardancy, the presence of amino and hydroxyl groups makes the flame retardant have good miscibility with other polyol components, and reacts with isocyanate to combine flame retardant elements into the molecular structure of polyurethane go, greatly improving the durability of the flame retardant

Method used

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  • Halogen-free reaction type flame retardant for polyurethane foam as well as preparation method and application thereof
  • Halogen-free reaction type flame retardant for polyurethane foam as well as preparation method and application thereof
  • Halogen-free reaction type flame retardant for polyurethane foam as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Weigh 110 parts by mass of DOPO, 30 parts by mass of ethanolamine, and 15 parts by mass of paraformaldehyde, mix them evenly, heat up to a temperature of 90°C in a nitrogen atmosphere, and react for 4 hours. After the reaction is completed, remove the water in the solution to obtain a halogen-free reaction type flame retardant. Then according to the formula in Table 1, first mix the combined polyol, DOPO derivative halogen-free reactive flame retardant and additives evenly under high-speed stirring conditions, and then stir with isocyanate under high-speed stirring conditions for 10-20s at a speed of 2000 ~3000r / min, pour into the mold, and mature for 48h.

Embodiment 2

[0043] Weigh 100 parts by mass of DOPO, 35 parts by mass of monoethanolamine, and 35 parts by mass (37%wt) of formaldehyde solution and mix evenly, heat up to a temperature of 80°C in a nitrogen atmosphere, react for 5 hours, and remove the water in the solution after the reaction is complete The halogen-free reactive flame retardant can be obtained. Then according to the formula in Table 1, first mix the combined polyol, DOPO derivative halogen-free reactive flame retardant and additives evenly under high-speed stirring conditions, and then stir with isocyanate under high-speed stirring conditions for 10-20s at a speed of 2000 ~3000r / min, pour into the mold, and mature for 48h.

Embodiment 3

[0045] Weigh 105 parts by mass of DOPO, 45 parts by mass of diethanolamine, and 15 parts by mass of paraformaldehyde, mix them uniformly, heat up to a temperature of 90°C in a nitrogen atmosphere, and react for 5 hours. After the reaction is completed, remove the water in the solution to obtain Halogen reactive flame retardant. Then according to the formula in Table 1, first mix the combined polyol, DOPO derivative halogen-free reactive flame retardant and additives evenly under high-speed stirring conditions, and then stir with isocyanate under high-speed stirring conditions for 10-20s at a speed of 2000 ~3000r / min, pour into the mold, and mature for 48h.

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Abstract

The invention provides a halogen-free reaction type flame retardant for polyurethane foam as well as a preparation method and an application thereof. The halogen-free reaction type flame retardant is prepared through a Mannich reaction of 9,10-dihdro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO), alcohol amine and formaldehyde; the structural formula of the halogen-free reaction type flame retardant is as shown in the specification; the alcohol amine and the formaldehyde are introduced to the DOPO flame retardant structure through a DODO reaction; the cost of the flame retardant is reduced; the synthesized halogen-free reaction type flame retardant contains active hydroxyl, flame retardant nitrogen and phosphorus, and primary amine or tertiary amine and has relatively high reaction activity; as rigid benzene rings are applied to the flame retardant type polyurethane foam, the flame retardant type polyurethane foam has relatively high flame retardance, the strength and the flame retardance durability of the flame retardant type polyurethane foam are improved, and the oxygen index can reach 23-28%. The flame retardant type polyurethane foam has wide application prospect in buildings, heat preservation fields and certain special occasions.

Description

technical field [0001] The invention belongs to the technical field of halogen-free phosphorus-based flame retardants, and mainly relates to a halogen-free reactive flame retardant, a synthesis method thereof, and an application in flame-retardant rigid polyurethane foam. Background technique [0002] 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide is an excellent polyurethane foam flame retardant, which can be used in polyurethane foam insulation materials, 9,10-dihydro-9 -Oxa-10-phosphaphenanthrene-10-oxide (DOPO) and its derivatives have a biphenyl ring and a phenanthrene ring structure in their molecular structure, especially the side phosphorus group is introduced in the form of a ring O=P-O bond , higher thermal stability and chemical stability than ordinary, uncycled organic phosphates, and better flame retardancy. DOPO and its derivatives can be used as reactive and additive flame retardants. The synthesized flame retardants are halogen-free, smoke-free, non-toxi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/38C08G18/32C07F9/6574
CPCC07F9/657172C08G18/3889C08G18/66C08G2110/0025
Inventor 张猛周永红张立强
Owner 徐州市洛克尔化工科技有限公司
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