Phenyl phosphate flame retardant containing DOPO, and preparation method and application thereof

A technology of phenyl phosphate and flame retardants, applied in the field of phenyl phosphate flame retardants, can solve problems such as the inability to meet the processing temperature of polymer materials, and achieve the effects of easy industrial production, advanced technology, and high phosphorus content

Inactive Publication Date: 2015-07-15
湖北万锦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because DOPO and its derivatives contain biphenyl ring and phenanthrene ring structure in their molecular structure, especially the side phosphorus group is introduced in the form of cyclic O=P-O bond, it has higher thermal stability and chemical stability than non-cyclic organic phosphate , better flame retardant performance, and halogen-free, smoke-free, environmentally friendly, and not easy to migrate. However, DOPO monomers are directly used in the flame retardant of polymer materials and have the disadvantage of starting to decompose at 180°C, which cannot meet the processing temperature of most polymer materials.

Method used

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  • Phenyl phosphate flame retardant containing DOPO, and preparation method and application thereof
  • Phenyl phosphate flame retardant containing DOPO, and preparation method and application thereof
  • Phenyl phosphate flame retardant containing DOPO, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of DOPO-containing phenyl phosphate flame retardant, the steps are:

[0028] Add 13.10 g (0.12 mol) of 4-aminophenol, 14.66 g (0.12 mol) of 2-hydroxybenzaldehyde, 25.94 g (0.12 mol) of DOPO, and 250 mL of methanol into a flask equipped with a stirrer, a reflux condenser and a tail gas absorber. Nitrogen gas was introduced, and after 10 hours of reaction at room temperature, 9.84 g (0.12 mol) of 37% formaldehyde was added, and the reaction was carried out at room temperature for 6 hours. After the reaction, the reaction solution was poured into 300 mL of water, and a large amount of white solid was precipitated, which was filtered by suction and dried in vacuum to obtain Intermediate I with a yield of 91.2%.

[0029] In the flask equipped with stirrer, reflux condenser and tail gas absorbing device, add 50.64g (0.24mol) phenoxyphosphoryl dichloride, start stirring, 13.2g (0.12mol) resorcinol and 101.28g (0.48 mol) phenoxyphosphoryl dichloride was ad...

Embodiment 2

[0037] A preparation method of DOPO-containing phenyl phosphate flame retardant, the steps are:

[0038]Add 13.10 g (0.12 mol) of 4-aminophenol, 14.66 g (0.12 mol) of 2-hydroxybenzaldehyde, 25.94 g (0.12 mol) of DOPO, and 260 mL of acetonitrile into a flask equipped with a stirrer, a reflux condenser, and a tail gas absorption device. Nitrogen gas was introduced, and after 10 hours of reaction at room temperature, 9.84 g (0.12 mol) of 37% formaldehyde was added, and the reaction was carried out at room temperature for 6 hours. After the reaction, the reaction solution was poured into 300 mL of water, and a large amount of white solid was precipitated, which was filtered by suction and dried in vacuum to obtain Intermediate I with a yield of 91.2%.

[0039] In the flask equipped with stirrer, reflux condenser and tail gas absorbing device, add 50.64g (0.24mol) phenoxyphosphoryl dichloride, start stirring, 13.2g (0.12mol) resorcinol and 101.28g (0.48 mol) phenoxyphosphoryl dich...

Embodiment 3

[0043] A preparation method of DOPO-containing phenyl phosphate flame retardant, the steps are:

[0044] Add 13.10 g (0.12 mol) of 4-aminophenol, 14.66 g (0.12 mol) of 2-hydroxybenzaldehyde, 25.94 g (0.12 mol) of DOPO, and 250 mL of methanol into a flask equipped with a stirrer, a reflux condenser and a tail gas absorber. Nitrogen gas was introduced, and after 10 hours of reaction at room temperature, 9.84 g (0.12 mol) of 37% formaldehyde was added, and the reaction was carried out at room temperature for 6 hours. After the reaction, the reaction solution was poured into 300 mL of water, and a large amount of white solid was precipitated, which was filtered by suction and dried in vacuum to obtain Intermediate I with a yield of 91.2%.

[0045] In the flask equipped with stirrer, reflux condenser and tail gas absorbing device, add 50.64g (0.24mol) phenoxyphosphoryl dichloride, start stirring, 13.2g (0.12mol) resorcinol and 101.28g (0.48 mol) phenoxyphosphoryl dichloride was ad...

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Abstract

Preparation method and application of a phenyl phosphate flame retardant containing DOPO. The method is as below: under the action of methanol, reacting 4-amino phenol, 2-hydroxy benzaldehyde, DOPO and formaldehyde in one pot to synthesize an intermediate I; reacting phenyl dichlorophosphate and resorcinol to synthesize an intermediate II (resorcinol bisphenoxyl phosphoryl chloride); and reacting the intermediate I and intermediate II to obtain a white solid which is the phenyl phosphate flame retardant containing DOPO. The initial decomposition temperature of the flame retardant was about 363, and the rate of residual carbon was 49% at 468, 800, and the flame retardant had good thermal stability, high residual carbon ratio and good flame retardant effect, which can be used for the non halogen flame retardant of polypropylene and ABS.

Description

technical field [0001] The invention belongs to the technical field of phosphorus-nitrogen synergistic flame-retardant compounds, and specifically relates to a DOPO-containing phenyl phosphate flame retardant. The flame retardant has good thermal stability, high carbon residue rate, and good flame-retardant effect. Halogen-free flame retardant for polypropylene and ABS. Background technique [0002] Organophosphorus flame retardant is a flame retardant with good flame retardant performance. It has dual functions of flame retardant and plasticizing. It overcomes the hydrogen halide and other corrosive and The disadvantage of toxic thermal cracking products, especially DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) is a new type of flame retardant intermediate, which contains active phosphorus in its structure -Hydrogen bonds, react with compounds containing olefins, epoxy bonds and carbonyls to generate derivatives with unique properties. Because DOPO and its der...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C07F9/6574C08L23/12C08L55/02
Inventor 李德江刘义稳谢益碧
Owner 湖北万锦科技有限公司
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