Polyurethane foam fire retardant, and preparation method and applications thereof

A polyurethane foam and flame retardant technology, which is applied in the field of polyurethane foam flame retardants, can solve the problems of high cost of DOPO and restrictions on DOPO flame retardants, and achieve the effects of improving durability, improving compression performance, and reducing costs

Inactive Publication Date: 2013-11-06
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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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 aniline and benzaldehyde to DOPO, the cost of flame retardants can be greatly reduced, and benzene The presence of the ring enhan

Method used

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  • Polyurethane foam fire retardant, and preparation method and applications thereof
  • Polyurethane foam fire retardant, and preparation method and applications thereof
  • Polyurethane foam fire retardant, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Step 1: Mix 80-100 parts by mass of aniline and 100-110 parts by mass of benzaldehyde evenly, heat up to a temperature of 50-60° C. in a nitrogen atmosphere, and react for 4-6 hours. The quality of aniline can choose 80 parts, 84 parts, 88 parts, 92 parts, 96 parts, 100 parts, the quality of benzaldehyde can choose 100 parts, 102 parts, 104 parts, 106 parts, 108 parts, 110 parts, and the temperature can be selected 50°C, 52°C, 54°C, 56°C, 58°C, 60°C, the reaction time can be selected from 4h, 4.5h, 5h, 5.5h, 6h.

[0049] Step 2: Mix 40-60 parts by mass of raw material 2-[(phenyliminomethyl)]benzene, 60-80 parts by mass of DOPO, and 450-500 parts by mass of tetrahydrofuran obtained in step 1. Under the environment of 50~70℃, react for 11~12h. The mass parts of 2-[(phenyliminomethyl)]benzene obtained in step 1 can be selected from 40 parts, 44 parts, 48 ​​parts, 52 parts, 56 parts, and 60 parts, and DOPO can be selected from 60 parts, 64 parts, and 68 parts , 72 parts, ...

Embodiment 2

[0051] Weigh 80 parts by mass of aniline and 100 parts by mass of benzaldehyde and mix them uniformly, heat up to 50°C in an atmosphere of nitrogen gas, and react for 4h to obtain 2-[(phenyliminomethyl)]benzene. Methanol crystallized. Weigh 40 parts by mass of the intermediate product 2-[(phenyliminomethyl)]benzene, 60 parts by mass of DOPO, and 500 parts by mass of tetrahydrofuran, mix them uniformly, and react at 50° C. for 11 h in a nitrogen atmosphere. The flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene was obtained by washing with cold tetrahydrofuran three times. Then according to the formula in Table 1, firstly mix the phthalic anhydride polyol and additives evenly under high-speed stirring, then ultrasonically mix for 30 minutes, and then stir with isocyanate under high-speed stirring for 20-30s at a speed of 2000-3000r / min, pour Put it into the mold and mature for 48 hours.

Embodiment 3

[0053] Take by weighing 80 parts by mass of aniline and 102 parts by mass of benzaldehyde and mix them uniformly, heat up to a temperature of 50° C. in an atmosphere of nitrogen, and react for 4.5 hours to obtain 2-[(phenyliminomethyl)]benzene. Crystallization from cold methanol. Weigh 40 parts by mass of the intermediate product 2-[(phenyliminomethyl)]benzene, 64 parts by mass of DOPO, and 500 parts by mass of tetrahydrofuran, mix them uniformly, and react at 54° C. for 11.2 h in a nitrogen atmosphere. The flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene was obtained by washing with cold tetrahydrofuran three times. Then according to Table 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline) methyl] benzene flame-retardant rigid polyurethane foam Alcohol, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene and additives were mixed evenly under high-speed stirring, and then ultrasonic Mix for ...

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Abstract

The invention discloses a polyurethane foam fire retardant obtained by reacting 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, aniline and benzaldehyde. The structural formula of the polyurethane foam fire retardant is represented by a formula in the patent specification. According to the preparation method of 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene, aniline and benzaldehyde are introduced into the 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) fire retardant structure by Mannich reaction, so that the cost of the fire retardant is reduced; synthesized 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene is used as a fire-retardant rigid polyurethane foam, and possesses relatively high fire retardant; and the oxygen index can reach 24 to 26%. The polyurethane foam fire retardant possesses a promising application prospect in buildings, insulation, and specific occasions.

Description

technical field [0001] The invention belongs to the technical field of polyurethane foam flame retardants, and mainly relates to 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide-4-[(aniline)methyl]benzene flame retardants Synthesis method and its 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 h...

Claims

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Application Information

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IPC IPC(8): C08K5/5313C07F9/6574C08G18/38
Inventor 周永红张立强张猛胡丽红杨晓慧
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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