Synthesis and application of reaction type halogen-free phosphorus-containing flame retardant for polyurethane

A reactive, flame retardant technology, applied in the application field of the phosphorus-containing flame retardant in polyurethane, can solve the problems of easy decomposition, not yet seen, etc., and achieves easy availability of raw materials, good dimensional stability, and mild reaction conditions. Effect

Active Publication Date: 2014-06-04
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the flame retardant is a glassy solid at room temperature, and it is an additive type flame retardant, which has the disadvantage of being easy to decompose during processing.
[0004] From the c

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0029] Example 1 Synthesis of phosphorus-containing monomer derivatives.

[0030] Example 1

[0031] Add 86.4 parts of phosphorus-containing monomer (DOPO) to the solvent, heat to 70°C, and after it is completely dissolved, add 46.4 parts of maleic acid and dissolve, and react at 100°C for 18h to obtain a phosphorus-containing monomer derivative. The yield of phosphorous monomer derivatives was 78.2%, and the acid value was 333.2 mgKOH / g.

Example Embodiment

[0033] Example 2

[0034] Add 72.2 parts of diethylene glycol to 132.8 parts of phosphorus-containing monomer derivatives, then add 0.8 parts of tetrabutyl titanate, a certain amount of water-carrying agent, and gradually increase the temperature at 140℃-200℃, and react for 18h. Reduce the acid value to below 2mgKOH / g, then vacuum remove the water-carrying agent and excess small molecular alcohol in the system to obtain a light yellow transparent viscous liquid. The thus synthesized phosphorus-containing flame retardant has a functionality of 2, a hydroxyl value of 127 mgKOH / g, and a molecular weight of 871 g / mol.

Example Embodiment

[0035] Example 3

[0036] Add 50.6 parts of glycerol to 83 parts of phosphorus-containing monomer derivatives, then add 0.7 parts of tetraisopropyl titanate, a certain amount of water-carrying agent, and gradually increase the temperature at 140℃-200℃, and react for 18h to make the acid The value is reduced to less than 2mgKOH / g, and then the water-carrying agent and excess small molecular alcohol in the system are removed under vacuum to obtain a light yellow transparent viscous liquid. The thus synthesized phosphorus-containing flame retardant has a functionality of 4, a hydroxyl value of 470 mgKOH / g, and a molecular weight of 477 g / mol.

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Abstract

The invention discloses synthesis and application of a reaction type halogen-free phosphorus-containing flame retardant for polyurethane. A phosphorus-containing monomer derivative is formed by a phosphorus-containing monomer 9, 10-dihydro-9-oxa-10-phospha- phenanthrene-10-oxide (DOPO) and unsaturated polycarboxylic acid or anhydride, further the phosphorus-containing monomer derivative and polyhydric alcohols are subjected to esterification reaction so as to form the reaction type halogen-free phosphorus-containing flame retardant which is liquid at a room temperature, the molecular weight of the flame retardant is 300-1000g/mol, a terminal group of the flame retardant is a hydroxide radical, and the degree of functionality of the flame retardant is 2-6. The application shows that the flame retardant has a very good compatibility with a polyurethane raw material system and can be mixed with a polyurethane raw material in any proportion. The flame retardant is used for preparing rigid polyurethane foam with the density of about 31kg/m<3> and has relatively good compression strength and high-low temperature size stability. The oxygen index of the polyurethane foam is increased to 23.9% from 19.2% of oxygen index of a blank sample; and the oxygen index of polyisocyanurate foam is increased to 25.2% from 20.3% of oxygen index of a blank sample. The flame retardant can be applied to the fields of rigid polyurethane foam, elastomers, synthetic leather slurry and the like.

Description

technical field [0001] The invention relates to the synthesis of a reactive halogen-free phosphorus-containing flame retardant for polyurethane and the application of the phosphorus-containing flame retardant in polyurethane. Background technique [0002] Polyurethane is a material with relatively comprehensive properties, which has the advantages of good physical and mechanical properties, excellent weather resistance and elasticity. At present, the total output of polyurethane in the world has exceeded 10 million tons, and its output and variety are increasing year by year. However, polyurethane is flammable in air and presents a certain fire hazard. Therefore, the research on flame retardant technology of polyurethane materials has attracted more and more people's attention. [0003] The molecular structure of DOPO contains biphenyl ring and phenanthrene ring structure, which has higher thermal stability and chemical stability than organic phosphate without ring formati...

Claims

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Application Information

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IPC IPC(8): C08G18/32C07F9/6574C08G18/66D06N3/14C08G101/00
CPCC07F9/65744C08G18/388C08G2110/0025D06N3/14D06N2203/068D06N2209/067D06N2211/28
Inventor 张杰付双徐勉
Owner EAST CHINA UNIV OF SCI & TECH
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